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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008



# Annex B



# Spirotetramat

B.7 Residue data

Reviewed by:

PMRA, Canada (B.7.1, B.7.2, B.7.3, B.7.5, B.7.7.2.1, B.7.8, B.7 .9, Annex II) AGES, Austria , (B.7.4, B.7.5, B.7.6, B.7.7.1, B.7.7.2.2, B.7.10, B.7.11, B.7.12,

B.7.13, B.7.14, B.7.15, B.7.16, Annex I)

PSD, UK (Annex III)

Peer – reviewed by: US EPA, USA PMRA, Canada AGES, Austria

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

B.7 Residue data.......................................

................................................... ..................................1

B.7.1 Metabolism, distribution and expression of residues in plants (Annex IIA 6.2; Annex

IIIA, 8.1) .........................................

................................................... ........................................5 B.7.1.1 Metabolism in cotton...............................

................................................... ...............................5 B.7.1.2 Metabolism in lettuce ..............................

................................................... ...............................9 B.7.1.3 Metabolism in potato...............................

................................................... .............................10 B.7.1.4 Metabolism in apple................................

................................................... .............................12 B.7.1.5 Overall conclusion on the metabolic fate on crops..

................................................... ............14 B.7.2 Metabolism, distribution and expression of residues in livestock (Annex IIA 6.2; Annex

IIIA, 8.1) .........................................

................................................... ......................................16 B.7.2.1 Metabolism in lactating goat .......................

................................................... .........................16 B.7.2.2 Metabolism in laying hen ...........................

................................................... ..........................18 B.7.2.3 Overall conclusion on the metabolic fate in livesto ck animals:........................................ .......19 B.7.3 Definition of the residue (Annex IIA 6.7; Annex III A 8.7) ............................................. ...........25 B.7.4 Use pattern for European Trials....................

................................................... .......................25 B.7.5 Intended uses of spirotetramat i.e. supported uses for evaluation under Directive

91/414/EEC and for NAFTA ...........................

................................................... .....................27 B.7.6 Residues resulting from supervised trials (Annex II A 6.3; Annex IIIA 8.3)............................. 38 B.7.6.1 Citrus fruits......................................

................................................... .....................................38 B.7.6.2 Lettuce ............................................

................................................... .....................................45 B.7.6.3 Pome fruit.........................................

................................................... ....................................51 B.7.6.4 Stone fruit........................................

................................................... .....................................58 B.7.6.4.1 Peach and apricot..................................

................................................... ..............................58 B.7.6.4.2 Plum...............................................

................................................... ......................................63 B.7.6.4.3 Cherry .............................................

................................................... .....................................67 B.7.6.5 Berries and small fruits ...........................

................................................... .............................71 B.7.6.5.1 Grapes .............................................

................................................... ....................................71 B.7.6.5.2 Strawberry.........................................

................................................... ...................................75 B.7.6.6 Bulb vegetable .....................................

................................................... ................................80 B.7.6.6.1 Onion ..............................................

................................................... .....................................80 B.7.6.7 Fruiting vegetables................................

................................................... ...............................84 B.7.6.7.1 Tomato.............................................

................................................... ....................................84 B.7.6.7.2 Pepper .............................................

................................................... ....................................88 B.7.6.7.3 Cucumber ...........................................

................................................... .................................94 B.7.6.7.4 Melons .............................................

................................................... ....................................99 B.7.6.8 Brassica vegetables................................

................................................... ...........................105 B.7.6.8.1 Flowering brassica.................................

................................................... ............................105 B.7.6.8.2 Head brassica......................................

................................................... ..............................110 B.7.6.8.3 Leafy brassica.....................................

................................................... ...............................118 B.7.6.8.4 Kohlrabi...........................................

................................................... ...................................122 B.7.6.9 Green bean (fresh, with pods) ......................

................................................... .....................126 B.7.6.10 Hops...............................................

................................................... ....................................128 B.7.6.11 Overall conclusion.................................

................................................... .............................132 B.7.6.12 Stability of residues prior to analysis ............

................................................... .....................133 B.7.6.12.1 Storage stability in plant commodities .............

................................................... ..................133 B.7.7 Effects of industrial processing and/or household p reparation (Annex IIA 6.5; Annex

IIIA 8.5) ..........................................

................................................... ....................................138 B.7.7.1 Effects on the nature of the residue...............

................................................... ....................138 B.7.7.1.1 BYI 08330 ..........................................

................................................... ................................138 B.7.7.1.2 BYI 08330-enol .....................................

................................................... .............................140

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

B.7.7.1.3 BYI 08330-enol-glucoside...........................

................................................... .......................142 B.7.7.1.4 BYI 08330-keto-hydroxy .............................

................................................... .......................144 B.7.7.1.5 BYI 08330-mono-hydroxy.............................

................................................... .....................147 B.7.7.2 Residue levels - balance studies on set of represen tative processes..................................1 49 B.7.7.2.1 Residue levels - balance studies on set of represen tative processes with relevance for

PMRA (Canada) and USEPA: ...........................

................................................... ................149 B.7.7.2.2 Residue levels - balance studies on set of represen tative processes with relevance for

the European Community (EU)........................

................................................... ..................158 B.7.8 Livestock feeding studies (Annex IIA 6.4; Annex III A 8.4)............................................. .......188 B.7.9 Residues in succeeding crops or rotational crops (A nnex IIA 6.6; Annex IIIA 8.6) ..............192 B.7.9.1 Confined rotational crop study using radiolabelled material........................................... ......192 B.7.9.2 Crop rotation studies (field test).................

................................................... ........................197 B.7.9.3 Overall conclusion.................................

................................................... .............................200 B.7.10 Proposed pre-harvest intervals for envisaged uses, or withholding periods, in the case

of post harvest uses (Annex IIA 6.8; Annex IIIA 8.8 ).................................................. ..........200 B.7.11 Community MRL and MRLs in EU Member States (Annex I IIA 11.2)..................................201

B.7.12 Proposed EU MRLs and justification for the acceptab ility of those MRLs (Annex IIA

6.7; Annex IIIA 8.7) ...............................

................................................... .............................201 B.7.12.1 Food of animal origin ..............................

................................................... ...........................201 B.7.13 Proposed EU import tolerances and justification for the acceptability of those residues.....202

B.7.14 Basis for differences, if any, in conclusions reach ed having regard to established or

proposed CAC MRLs..................................

................................................... .......................203 B.7.15 Estimates of potential and actual dietary exposure through diet and other means

(Annex IIA 6.9; Annex IIIA 8.10) ...................

................................................... .....................203 B.7.15.1 Estimation of the potential and actual exposure thr ough diet.......................................... .....203 B.7.15.2 Estimation of chronic exposure through diet ........

................................................... .............203 B.7.15.2.1 Estimation of acute exposure through diet ..........

................................................... ..............204 B.7.15.3 Estimation of the potential and actual exposure thr ough other means ................................205 B.7.16 Summary and evaluation of residue behaviour (Annex IIA 6.11.1; Annex IIIA 8.11) ...........205

B.7.17 References relied on...............................

................................................... ...........................212 Annex I a: Summary of trial information – citrus fr uits............................................... .....................................247 Annex I b: Summary of trial information - lettuce ..

................................................... ......................................253 Annex I c: Summary of trial information – pome frui t .................................................. ...................................258 Annex I d: Summary of trial information – Peach and apricot........................................... .............................263 Annex I e: Summary of trial information – Plum.....

................................................... .....................................266 Annex I f: Summary of trial information – Cherry ...

................................................... .....................................269 Annex I g: Summary of trial information – Grapes ...

................................................... ...................................272 Annex I h: Summary of trial information – Strawberr y.................................................. ..................................275 Annex I i: Summary of trial information – Onion....

................................................... ......................................278 Annex I j: Summary of trial information – tomato ...

................................................... .....................................281 Annex I k: Summary of trial information – pepper ...

................................................... ....................................284 Annex I l: Summary of trial information – cucumber .

................................................... ..................................288 Annex I m: Summary of trial information – melon ....

................................................... ...................................291 Annex I n: Summary of trial information – flowering brassica .......................................... ..............................297 Annex I o: Summary of trial information – Brussels sprouts ............................................ ..............................300 Annex I p: Summary of trial information – round cab bage, red cabbage and savoy cabbage ................ ......302 Annex I q: Summary of trial information – leafy bra ssica .............................................. .................................305 Annex I r: Summary of trial information – kohlrabi .

................................................... .....................................307 Annex I s: Summary of trial information – green bea ns ................................................. ................................309 Annex I t: Summary of trial information – hop ......

................................................... .......................................311 Annex II – Summary of trials conducted in NAFTA Reg ions............................................... ...........................313

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Annex III: Import tolerances (evaluation document o f UK):............................................. ...............................336

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

B.7.1 Metabolism, distribution and expression of re sidues in plants (Annex IIA 6.2; Annex

IIIA, 8.1)

B.7.1.1 Metabolism in cotton

Reference: Metabolism of [azaspirodecenyl-3-14C]BYI 08330 in c otton after spray application Author(s), year: Spiegel, K. 2006 Report/Doc. number: Report No.: MEF-236/04, Edition Number: M-269105-01-2 Guideline(s): PMRA Regulatory Directive 98-02; DACO 6.3; EPA OPTTS 860.1300 GLP: Yes. Deviations: No. Validity: Yes.

Material and methods :

The metabolism of spirotetramat was investigated in cotton (gin trash, lint & undelinted seeds) follow ing two spray applications of [azaspirodecenyl-3- 14 

### C]-spirotetramat, formulated as a suspension concen trate (240 SC), at a total rate of 264 g a.i./ha/season (0.23 lbs. a.i./A)). The first application was made at a n early growth stage (BBCH 15) at a rate of 91.7 g a.i./ha, and the second at growth stage 85 (134 days interv al) at a rate of 172.3 g a.i./ha. One immature cotton pla nt sample was collected at 19 days after the first application. Cotton gin trash, lint and undelinted seed samples were harvested 39 days after the last

treatment.

Intermediate samples, gin trash, lint and undelinte d seed underwent homogenization and successive extractions with acetonitrile (ACN)/water (lint und erwent a final extraction with ACN only). Aliquots of combined extracts were subjected to analysis by liq uid scintillation counting (LSC). The remaining so lids were air dried, and aliquots were combusted and mea sured for radioactivity using LSC. TRR values were calculated by combining the radioactivity detected in the extracts and solids. Further analysis was undertaken in which the ACN/water extracts were par titioned with dichloromethane (DCM) to yield an organic and aqueous phase. Each phase was measured for radioactivity using LSC and analyzed by highperformance liquid chromatography (HPLC). Fractions containing the purified metabolites were concentra ted and analyzed by HPLC-mass spectrometry (MS)/MS and/ or Fourier Transform (FT)-MS. Resulting conjugates were identified by HPLC and/or thin-laye r chromatography (TLC) analysis. The conjugates of the intermediate sample were cleaved by acidic treatmen t and enzymatic hydrolysis with ß-glucosidase.

Findings :

The total radioactive residue (TRR) was 2.381 mg-eq uiv./kg in the immature plant sample, 1.641 mgequiv./kg in gin trash, 1.078 mg-equiv./kg in lint, and 0.119 mg-equiv./kg in undelinted seed. Parent compound, spirotetramat, was the major residue (46. 95% of the TRR, 1.117 mg-equiv./kg) identified in t he immature cotton plant. Also identified were 13 minor metabolites ranging f rom 0.18% to 9.76% of the TRR (0.004-0.232 mgequiv./kg). The major residues identified in cotton gin trash were BYI 08330-ketohydroxy (29.7% of the TRR; 0.478 mg-equiv./kg), spirotetramat (19.8% of the TR R; 0.319 mg-equiv./kg), and BYI 08330-enol (12.1% o f the TRR; 0.196 mg-equiv./kg). The major residues i dentified in cotton lint were spirotetramat (32.3% of the TRR; 0.348 mg-equiv./kg), BYI 08330-mandelic acid a mide (11.9% of the TRR; 0.128 mg-equiv./kg), and BYI 08330-ketohydroxy (10.5% of the TRR; 0.113 mg-e quiv./kg). The major residue found in the cotton undelinted seeds was BYI 08330-enol (39.8% of the T RR; 0.047 mg-equiv./kg), while BYI 08330-

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

ketohydroxy represented 9.04% of the TRR (0.011 mg- equiv./kg). Ten metabolites representing 0.6-4.4% of the TRR (0.003-0.064 mg-equiv./kg) were also identi fied in the gin trash, lint and undelinted seeds.- 7 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Table B.7.1.1-1: Summary of Characterization and Identification of Radioactive Residues in Plant Matrices Following Application of RadiolabeledSpirotetramat at 264 g a.i./ha.Intermediate Gin Trash Lint Undelinted SeedTRR=2.381mg-equiv./kgTRR=1.614mg-equiv./kgTRR=1.078mg-equiv./kgTRR=0.119mg-equiv./kgTRR=2.381mg-equiv./kgTRR=1.614mg-equiv./kgTRR=1.078mg-equiv./kgTRR=0.119mg-equiv./kgMetabolite Fraction%TRR mg-equiv./kg %TRR mg-equiv./kg %TRR mg-equiv./kg %TRR mg-equiv./kg-enol-Glc 4.65 0.111 - - - - - --mandelic acid - - - - 0.89 0.010 - --mandelic acid amide 0.36 0.009 1.65 0.027 11.87 0.128 1.30 0.002-desmethyl-enol-Glc 3.82 0.091 1.75 0.028 - - 3.460.004-desmethyl-ketohydroxy-Glc(I1)3.45 0.082 1.42 0.023 0.14 0.001 - --desmethyl-ketohydroxy-Glc(I2)6.31 0.150 2.32 0.038 - - - --hydroxymorpholinedion 0.61 0.014 0.64 0.01 - - - --desmethyl-ketohydroxy 0.18 0.004 0.56 0.009 - - ---MA-amide 0.58 0.014 1.54 0.025 4.12 0.044 - --enol 1.98 0.047 12.09 0.196 9.46 0.101 39.8110.0471-ketohydroxy 5.40 0.129 29.65 0.478 10.45 0.113 9.04 0.011BYI 08330-olefine(I1) 0.54 0.013 1.76 0.028 4.08 0.044 - -BYI 08330-olefine(I2) 0.43 0.010 2.04 0.033 4.35 0.047 - -Spirotetramat (a.i.) 46.94 1.117 19.78 0.319 32.320.348 0.42 <0.001Total Identified (conventionalextraction methods)75.3 1.791 79.2 1.278 77.7 0.837 22.9 0.027Total Identified afterexhaustive extraction methods- - - - - - 34.6 0.041Total Identified Overall 75.3 1.791 79.2 1.278 77.70.837 57.5 0.068Total Characterized 8.8 0.210 9.4 0.152 14.8 0.16013.9 0.017Not Analyzed - - - - - - 9.1 0.011Total Extractable 84.1 2.002 88.6 1.430 92.5 0.99780.5 0.096Total Bound115.9 0.379 11.4 0.184 7.5 0.080 9.6 0.011Precipitate - - - - - - 9.9 0.012Total/Accountability 100.0 2.381 100.0 1.614 100.01.078 100 0.1191Residues remaining after exhaustive extractions.2Accountability = (Total extractable + Total unextractable)/(TRR from combustion analysis) * 100.- 8 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008#Divides into 4 different phases obtained during partitioning and clean-up, none of the phase exceeded0.005 mg-equiv./kg; the compounds in the phases are characterizedby their partitioning behaviour and/or their retention behaviour on an RP18 column.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Conclusion : The major metabolic step for spirotetramat in cotto n involved the hydrolysis of the ethyl carbonate gr oup to form BYI 08330-enol. Oxidation of the pyrroline mo iety of BYI 08330-enol led to the formation of BYI 08330- ketohydroxy. Cleavage of the pyrroline ring of BYI 08330-ketohydroxy followed by decarboxylation and hydrolysis yielded BYI 08330-MA-amide, BYI 08330-ol efin, BYI 08330-mandelic acid amide, and BYI 08330- mandelic acid. Demethylation of the cyclohexyl met hoxy group of BYI 08330-enol and BYI 08330- ketohydroxy and conjugation led to the formation of BYI 08330-desmethyl-ketohydroxy and the glucoside and BYI 08330-desmethyl-enol-glucoside. Other mino r metabolic reactions involved ring closure of BYI 08330-MA-amide to form a morpholine ring and conjug ation of BYI 08330-enol with glucose.

Comments (RMS): None.

B.7.1.2 Metabolism in lettuce

Reference: Metabolism of [azaspirodecenyl-3-14C]BYI08330 in le ttuce Author(s), year: Haas, M., Diederich, B. 2004. Report/Doc. number: Report No.: MEF-049/04, Edition Number: M-242667-01-2 Guideline(s): PMRA Regulatory Directive 98-02; DACO 6.3; EPA OPTTS 860.1300 GLP: Yes Deviations: No Validity: Yes

Material and methods :

The metabolism of spirotetramat was investigated in head lettuce following two spray applications of [azaspirodecenyl-3- 14 

### C]-spirotetramat, formulated as an oil-dispersion f ormula (100 OD), at a total rate of 167 g a.i./ha (0.15 lbs a.i./A). The two applicati ons were made at a 14-day retreatment interval. Tr eated lettuce was harvested at maturity 7 days after the last treatment.

Lettuce plants were harvested by cutting directly a bove the soil. Heads were weighed and cut into sma ller pieces using garden secateurs and homogenized in li quid nitrogen. Homogenized sample material was separated into aliquots and stored at -20oC. Immedi ately following harvest, a first extraction was per formed. Aliquots of homogenized lettuce were successively e xtracted with ACN/water (80/20, v/v). After each extraction, the suspension was centrifuged. Extrac ts were measured for radioactivity by liquid scinti llation counting (LSC), after which they were combined and concentrated. The remaining lettuce solids were ai rdried and aliquots were combusted and radioactivity was measured by LSC.

TRRs were calculated as the sum of the three extrac ts and the solids. Further analysis of extracts wa s performed by combining and concentrating the ACN/wa ter extracts and partitioning them successively wit h dichloromethane (DCM), resulting in an organic and an aqueous phase. The phases were measured for radioactivity via LSC and analyzed by high-performa nce liquid chromatography (HPLC). An aliquot of the remaining solids was exhaustively extracted with AC N/water (1:1) for 30 minutes at 120oC using a microwave MARSX (CEM method BYI 083304). The resul ting extract was filtered, measured for radioactivity, concentrated and analyzed by HPLC.

Five months after harvest, a larger aliquot of the homogenized lettuce was extracted as described abov e. Isolation of the major compound present in the aque ous phase was achieved by solid-phase extraction (SPE) clean-up using a Mega Bond Elut C18 cartridge , and HPLC using methods BD1103A4 to BD1103A6.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

The purified metabolite was concentrated and used f or structure elucidation by HPLC/mass spectrometry (MS)/MS and nuclear-magnetic resonance (NMR) spectr oscopy.

Aliquots of the aqueous remainder and the aqueous p hase meant for hydrolysis were transferred into reaction vials and brought to the respective pH wit h base or acid. Prior to analyses, the hydrolyzed samples were neutralized, centrifuged, concentrated and dil uted with water. Where possible, samples were dire ctly analyzed with HPLC. These procedures were used to release glucose conjugates.

Findings :

Greater than 95% of the total radioactive residue ( TRR) in lettuce was extracted with acetonitrile (ACN)/water. The TRR was 3.13 mg-equiv./kg, calcul ated by summing extracts and post extraction solids

. Over 91% of the extracted radioactivity was identif ied. Unchanged parent compound spirotetramat was t he major residue identified (55.9% of the TRR; 1.75 mg -equiv./kg), followed by BYI 08330-enol (17.8% of t he TRR; 0.56 mg-equiv./kg), BYI 08330-enol-glucoside ( 11.4% of the TRR; 0.36 mg-equiv./kg), and BYI 08330

- ketohydroxy (6.2% of the TRR; 0.2 mg-equiv./kg).

Table B.7.1.2-1: Summary of Characterization and Id entification of Radioactive Residues in Plant Matrices Following Application of Radiolabeled Spir otetramat at 167 g a.i./ha/season

Lettuce Heads TRR =3.13 mg-equiv./kg Compound % TRR mg-equiv./kg Spirotetramat 55.9 1.75 BYI 08330-ketohydroxy 6.2 0.20

BYI 08330-enol 17.8 0.56 BYI 08330-enol-glucoside 11.4 0.36

Total identified 91.4 2.87

Total characterized 7.3 0.22

Total extractable 98.7 3.09 Unextractable (PES) 1 1.3 0.04 Accountability 2 100.00 3.13

1 Residues remaining after extractions



### . 2 Accountability = (Total extractable + Total unextrac table)/(TRRs from combustion analysis).



### Conclusion:

The metabolism of spirotetramat in lettuce involved the hydrolytic cleavage of the ester bond of the p arent compound to form BYI 08330-enol and subsequent conj ugation to BYI 08330-enol-glucoside. Further hydroxylation in the tetramic acid moiety resulted in BYI 08330-ketohydroxy.

B.7.1.3 Metabolism in potato

Reference: Metabolism of [azaspirodecenyl-3-14C]BYI 08330 in p otatoes Author(s), year: Sur, R., 2005 Report/Doc. number: Report No.: MEF-05/320, Edition Number: M-267707-01-2 Guideline(s): PMRA Regulatory Directive 98-02; DACO 6.3; EPA OPTTS 860.1300 GLP: Yes. Deviations: No. Validity: Yes.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Material and methods :

The metabolism of spirotetramat was investigated in potatoes (tuber & tops) following three spray applications of [azaspirodecenyl-3- 14 

### C]-spirotetramat, formulated as an oil dispersion ( 100 OD), at a total rate of 308 g a.i./ha (0.275 lbs. a.i./A). The app lications were made at a 21-day re-treatment interv al (RTI). Potato samples were harvested 14 days after the las t treatment.

Aliquots of tubers and tops were extracted three ti mes with ACN/water (4:1, v/v) and once with ACN. Extracts were filtered and the solids were washed w ith small amounts of ACN. Corresponding extracts w ere combined for determination of radioactivity by LSC. Undissolved solids were air dried yielding solids samples for radioactivity determination via combust ion and LSC. The results of the combined extracts and the solids were used in the calculation of the TRR. Further analysis was performed in which the combi ned extracts of tubers and tops were partitioned three times with dichloromethane (DCM), yielding an organ ic and an aqueous phase. Organic and aqueous phases w ere analyzed by high-performance liquid chromatography (HPLC) for quantitation of parent co mpound and metabolites. A second aliquot of tuber was extracted and partitioned with DCM for the isol ation of metabolites from the aqueous phase. TLC wa s employed for the sub-quantitation of metabolites in fractions collected from HPLC and for the identifi cation of metabolites by co-chromatography with reference com pounds.

Solids resulting from the first extraction of tuber s were further extracted by treatment with diastase . Aliquots of solids were incubated in a round bottomed flask with 22 mL of a diastase containing solution. The mixture was stirred for 6 days at room temperature. Afterw ards, it was centrifuged and the supernatant was decanted. The solid residue was extracted again in the same manner. Both supernatants were combined and aliquots were analyzed by HPLC and LSC. Undiss olved residues were air dried at room temperature resulting in a secondary set of solids for radioact ive analysis via combustion and LSC.

The enzyme cellulose (1.7 U/mg, type “Onozuka R-10” from the fungus Trichoderma viride ) was used to selectively cleave the O -1,4 glycoside bond of BYI 08330-desmethyl-enol-gly coside and BYI 08330- ketohydroxy-alcohol-glycoside to identify the corre sponding aglycons. Additionally, the aqueous phase of the tubers was also treated with cellulose. For ea ch test, solutions of cellulose were prepared and t ested for activity using p-nitrophenyl-ß-D-glucopyranoside. Sodium azide at 0.02% was added to minimize microbi al proliferation. Aliquots of the isolated conjugates or of the aqueous phase were evaporated to dryness and reconstituted with the cellulose containing solutio n or only with buffer (control sample).

Findings :

Approximately 80% of the total radioactive residue (TRR) in tuber, and 96% of the TRR in tops were extracted with acetonitrile (ACN)/water. Enzymatic treatment of the extracted tuber released approxim ately 14% of the TRR. The TRR in tuber and tops was 0.25 5 mg-equiv./kg and 11.057 mg-equiv./kg, respectivel y, calculated by summing extracts and post extraction solids.

Parent spirotetramat was not identified in potato t uber. The predominant metabolite identified was BYI 08330-enol (65.8% of the TRR; 0.168 mg-equiv./kg), followed by BYI 08330-ketohydroxy (6.8% of the TRR; 0.018 mg-equiv./kg) and BYI 08330-desmethyl-enol (6 .7% of the TRR; 0.018 mg-equiv./kg) and several other minor metabolites (≤2.5 % of the TRR; 0.006 m g-equiv./kg). In potato tops, spirotetramat and BYI 08330-ketohydroxy were the major residues identifie d, represented 49.4% (5.5 mg-equiv./kg) and 24.8% o f the TRR (2.7 mg-equiv./kg), respectively. BYI 0833 0-enol (7.8% of the TRR; 0.87 mg-equiv./kg) and sev eral other minor metabolites (≤3.6% of the TRR) were als o identified.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.1.3-1: Summary of Characterization and Id entification of Radioactive Residues in Plant Matrices Following Application of Radiolabeled Spir otetramat at 308 g a.i./ha/season. Tubers Tops TRR = 0.255 mg-equiv./kg TRR = 11.057 mg-equiv./kg Compound % TRR mg-equiv./kg % TRR mg-equiv./kg Spirotetramat ND ND 49.4 5.455

BYI 08330-enol 65.8 0.168 7.8 0.870 BYI 08330-enol-glucoside 2.5 0.006 3.6 0.395 BYI 08330-desmethyl-enol 6.7 0.018 1.1 0.119 BYI 08330-desmethyl-enol-glycoside 1.5 0.004 0.5 0.0 55 BYI 08330-enol-alcohol 0.6 0.002 0.2 0.020 BYI 08330-ketohydroxy 6.8 0.018 24.8 2.745 BYI 08330-ketohydroxy-alcohol 0.5 0.001 ND NDBYI 08330-ketohydroxy-alcoholglycoside 0.5 0.001 ND ND

BYI 08330-dihydroxy 0.2 0.001 ND ND

Total identified 85.1 0.217 87.4 9.659

Total characterized 9.4 0.024 8.7 0.957

Total extractable 94.5 0.241 96.0 10.616 Unextractable (PES) 1 5.5 0.014 4.0 0.442 Accountability 2 100 0.255 100 11.058 1 Residues remaining after extractions. 2 Accountability = (Total extractable + Total unextr actable)/(TRRs from combustion analysis).

ND Not detected



### Conclusion :

The metabolism of spirotetramat in potatoes mainly involved the hydrolysis of the parent compound to B YI 08330-enol, followed by the oxidation of BYI 08330- enol to BYI 08330-ketohydroxy. Further conjugation of BYI 08330-enol to BYI 08330-enol glucoside occurred with subsequent O -Demethylation of BYI 08330-enol to BYI 08330 desmethyl-enol.

B.7.1.4 Metabolism in apple

Reference: Metabolism of (azaspirodecenyl-3-14C)BYI08330 in ap ple after spray application Author(s), year: Haas, M.; Henk, F., 2005 Report/Doc. number: Report No.: MEF-028/04, Edition Number: M-244827-01-3 Guideline(s): PMRA Regulatory Directive 98-02; DACO 6.3; EPA OPTTS 860.1300 GLP: Yes. Deviations: No. Validity: Yes.

Material and methods :

The metabolism of spirotetramat was investigated in apple (fruits & leaves) following two spray applic ations of [azaspirodecenyl-3- 14 

### C]-spirotetramat, formulated as an oil-dispersion f ormula (100 OD), at a total rate of 1100 g a.i./ha (0.982 lb a.i./A). The first applica tion was at a growth stage 69 of the current BBCH c ode and the second application was 20 days later at growth stage 71, 2 months (63 days) before harvest. A supplementary apple cell culture study was also sub mitted. This study was conducted to ascertain the

### - 13 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

metabolic fate of spirotetramat in isolated plant c ells. As well, from this study, selected metabolit es were obtained in larger amounts to be used as radioactiv e reference compounds in guideline nature of the re sidue studies.

Apples were surface washed using dichloromethane (D CM). Aliquots of wash solution were concentrated and used for radioactive measurements using high-pe rformance liquid chromatography (HPLC) analysis. Surface washed apples were homogenized and stored f rozen until extraction. Aliquots of homogenate wer e extracted with ACN:water (80/20, v/v). After each extraction step, suspensions were filtered and filt ers were washed with ACN. Extracts were measured for radioa ctivity by liquid-scintillation counting (LSC), com bined and concentrated. The solids were lyophilized and aliquots of the homogenized solids were combusted a nd measured for radioactivity by LSC. Structure elucid ation was achieved by HPLC/mass spectrometry (MS)/MS and nuclear-magnetic resonance (NMR) spectr oscopy.

Apple leaves were homogenized with liquid nitrogen and extracted three times with ACN/water (80/20, v/ v). At each step the leaves were macerated and filtered , after which the radioactivity of each extract was determined separately prior to being combined. Lea f solids were air-dried, subjected to combustion an d measured for radioactivity by LSC.

From the apple cell culture study, samples were tak en seven days after application of radiolabelled spirotetramat. Cells were separated from the nutri ent medium by filtration. The cells were washed intensively with water to remove soluble radioactiv ity from the cell surfaces. The wash solution was combined with the nutrient medium. Liquid samples were concentrated at 35oC and re-dissolved in an appropriate solvent for further investigation.

Findings :

Total radioactive residue (TRR) amounted to 0.61 mg -equiv./kg (apple) and 36.63 mg-equiv./kg (apple leaves). Approximately 49% of the TRR (0.3 mg-equi v./kg) in apple was surface residues washed with dichloromethane. Washed apple extracted with aceto nitrile (ACN)/water yielded 49.5% of the TRR leavin g only 2.1% of the TRR (0.01 mg-equiv./kg) as unextra ctable residues. Unchanged parent spirotetramat wa s the only residue detected in the surface wash. The predominant residue found in the extract was BYI 0 8330- mono-hydroxy followed by BYI 08330-ketohydroxy, BYI 08330-di-hydroxy, BYI 08330-desmethylketohydroxy, BYI 08330-enol, and the respective gly cosides thereof. As in apple fruits, the major res idue in apple leaves was the unchanged spirotetramat (72% o f the TRR). Other residues detected were BYI 08330

- ketohydroxy, BYI 08330-enol, and glycoside isomers of BYI 08330-desmethyl-ketohydroxy. A BYI 08330- ketohydroxy-formiate-glycoside was also detected. A pproximately 44% of the recovered radioactivity was found in the cells and ca. 56% in the nutrient medi um. The major part of the radioactivity present in the extracts of cells and nutrient medium partitioned i nto the organic phase (ethyl acetate). The formati on of bound residues observed was minimal (<1% of the rec overed radioactivity).

Table B.7.1.4-1: Summary of Characterization and Id entification of Radioactive Residues in Apple Matrices Following Target Application of Radiolabel ed Spirotetramat at 1152 g a.i./ha. Apple Fruit Apple Leaves TRR = 0.61 mg-equiv./kg TRR = 36.63 mg-equiv./kg Compound % TRR mg-equiv./kg % TRR mg-equiv./kg Spirotetramat (parent) 51.3 0.32 72.0 26.37 BYI 08330-ketohydroxy 7.7 0.05 3.0 1.09

BYI 08330-enol 2.1 0.01 11.6 4.26 BYI 08330-mono-hydroxy 15.6 0.10 ND ND BYI 08330-desmethyl-ketohydroxy 3.8 0.02 ND ND BYI 08330-di-hydroxy 4.4 0.03 ND ND

### - 14 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Apple Fruit Apple Leaves TRR = 0.61 mg-equiv./kg TRR = 36.63 mg-equiv./kg Compound % TRR mg-equiv./kg % TRR mg-equiv./kgBYI 08330-desmethyl-ketohydroxyglucoside (isomers), in leaves also +BYI 08330-ketohydroxy-formiate-glycoside 1.9 0.01 8.0 2.92

BYI 08330-enol-glycoside 5.1 0.03 ND ND

Total identified 91.9 0.57 94.6 34.65

Total characterized 6.0 0.04 ND ND

Total extractable 98.0 0.60 94.6 34.65 Unextractable (PES) 1 2.1 0.01 5.4 1.97 Accountability 2 100.0 0.61 100.0 36.63 1 Residues remaining after extractions. 2 Accountability = (Total extractable + Total unextr actable)/(TRRs from combustion analysis).

ND Not detected



### Conclusion :

Major reactions involved in the degradation of the parent compound were hydrolysis of the side chain e ster bond resulting in the BYI 08330-enol. A second hyd roxylation detected in the azaspiro moiety of this BYI 08330-enol gave the BYI 08330-keto-hydroxy. Demeth ylation of BYI 08330-enol resulted in the corresponding BYI 08330-4-hydroxyenol and further h ydroxylation correspondingly in the BYI 08330- hydroxy-keto-hydroxy metabolite. All metabolites w ere further conjugated to give mono and bis-glycosi des. In the supplemental study, the degradation of spiro tetramat was investigated in heterotrophic apple ce ll suspension cultures to ascertain the metabolic fate of spirotetramat in isolated plant cells. Spirote tramat was rapidly degraded by the apple cells to at least 14 compounds.

B.7.1.5 Overall conclusion on the metabolic fate on crops

The submitted metabolism data for apple, lettuce, c otton and potato are adequate to elucidate the natu re of the residue in plants. Major metabolic reaction in volved the hydrolytic cleavage of the carbonate est er parent bond of the parent compound to form BYI 0833 0-enol. Further reduction of the double bond in th e teramic acid moiety of BYI 08330-enol occurred to f orm the BYI 08330-mono-hydroxy metabolite. Hydroxylation in the tetramic acid moiety resulted in BYI 08330-ketohydroxy. Demethylation of the met hoxy group of the cyclohexyl ring resulted via a propose d intermediate (BYI 08330-desmethyl-enol) in BYI 08 330- desmethyl-ketohydroxy (after the corresponding hydr oxylation). Oxidation of the methoxy group resulte d in BYI 08330-ketohydroxy-formiate. Partly, metabolite s bearing a hydroxy group were conjugated with gluc ose.

In cotton, cleavage of the pyrrolidine ring of BYI0 8330-ketohydroxy followed by decarboxylation and fu rther cleavage reactions led to the formation of BYI08330 -MA-amide, BYI08330-olefin, BYI08330-mandelic acid amide, and BYI08330-mandelic acid. Ring closure of the initial cleavage product formed BYI08330- hydroxymorpholinedione.

### - 15 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Figure B.7.1.5-1: Proposed Metabolic Scheme in Plants

NH

O CH 3

CH 3 H OH

O O

HO HO

HO HO

BYI 08330- desmethyl-enol-Glc (C, P, Sc) CH 3

CH 3 NH

O H O

O O HO HO

HO HO

CH 3

BYI 08330- enol-Glc (C, P, A, Sc) NH

O CH 3

CH 3 H O CH 3 O O H 3 C O

BYI 08330 (parent)

e

*

NH

O CH 3

CH 3 H O CH 3

HO e

BYI 08330-enol (C, L, P, A, Sc) NH

O CH 3

CH 3 H OH

HO e

BYI 08330- desmethyl-enol (C, P, A, Sc)

CH 3

CH 3 NH

O HO H OH

OH

BYI 08330- dihydroxy (P, A) CH 3

CH 3 NH

O O H O

OH CH 3

BYI 08330- ketohydroxy (C, L, P, A, Sc)

e

BYI 08330-

ketohydroxyformiate (A) CH 3

CH 3 NH

O O H OH

OH

BYI 08330-desmethylketohydroxy (C, A, Sc)

e

CH 3

CH 3 NH

O O H OH

OH O

HO OH

OH

OH

OH +

-H 2 O

BYI 08330-desmethylketohydroxy-Glc (isomers) C, A, Sc)

BYI 08330-desmethylketohydroxy-bis-glycoside

(Sc) NH

O CH 3

CH 2 OH HO H O CH 3

BYI 08330- enol-alcohol (P)

CH 3 CH 3 NH HO O

O OH H O CH 3

BYI 08330- MA-amide (C) CH 3

CH 3 N

H H O

OH OCH 3

CH 3

CH 3 N H

OH O OCH 3

BYI 08330- olefine (C) CH 3

OH OH

CH 3 O

BYI 08330- mandelic acid (C)

CH 3

NH

2 OH

CH 3 O

BYI 08330- mandelic acid amide (C) CH 3

CH 2 OH NH

O O

OH H O CH 3

BYI 08330- ketohydroxy-alcohol (P) NH O

OH

CH 3 CH 3 O

O H O CH 3

BYI 08330- hydroxymorpholinedion (C)

CH 3

CH 2 OH NH

O O

OH H O CH 3

BYI 08330-ketohydroxy-alcoholglycoside (P)

+ C 6 H 12 O 6 - H 2 O CH 3

CH 3 NH

O HO H O CH 3 e

BYI 08330- mono-hydroxy (A)

BYI 08330-ketohydroxyformiate-glycoside (A)

+ hexose, -H 2 O CH 3

CH 3 NH

O O

OH H O C

H O e

### - 16 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

B.7.2 Metabolism, distribution and expression of re sidues in livestock (Annex IIA 6.2; Annex

IIIA, 8.1)

B.7.2.1 Metabolism in lactating goat

Reference: [Azaspirodecenyl-3-14C]BYI 08330: Absorption, distr ibution, excretion, and metabolism in the lactating goat Author(s), year: Koester, J., Klempner, A., 2006 Report/Doc. number: Report No.: MEF-05/293, Edition Number: M-269256-01-2 Guideline(s): PMRA Directive 98-02; DACO 6.2/EPA OP PTS 860.1300 GLP: Yes. Deviations: No. Validity: Yes.

Material and methods :

The nature of the residue in milk and foodstuffs or iginating from ruminants was investigated with a la ctating goat following 4 daily oral administrations of [aza spirodecenyl-3- 14 

### C]-spirotetramat at a mean dose rate of 2.22 mg a.i./kg bw/day (73.03 mg/kg in feed) given by gavage. Milk samples were collected twice daily

, urine and feces were collected once daily. The tre ated goat was sacrificed ca. 24 hrs after the last dosage, and muscle (round, flank, loin), fat (perirenal, om ental subcutaneous), liver, and kidneys were collec ted.

Liver, kidney, fat and muscle samples were homogeni zed 4-5 times in a half-frozen state using a mincin g machine. Aliquots of the resulting tissue pulp wer e weighed, freeze-dried, weighed again and homogeni zed prior to radioactivity measurement by combustion/LS C. Perirenal and omental fat also underwent the determination of total radioactivity by LSC after s olubilization of tissues with Beckman Tissue Solubi liser (BTS)-450. The gall bladder was dissected from the liver and punctured for the collection of bile.

Samples were extracted 3-4 times with acetonitrile (ACN): water. Extracts were combined and defatted by reversed-phase solid-phase extraction (SPE). Flow- through fraction and rinse solution were combined a nd concentrated. In the case of fat and kidney, the c oncentrates were directly analyzed by high-performa nce liquid chromatography (HPLC). All other concentrat ed aqueous extracts were further purified by partit ion and SPE clean-up procedures. In the case of liver, two final extracts were obtained for each sample w hich were analyzed separately by HPLC. TLC co-chromatogr aphy was used for confirmation of metabolites in isolated HPLC fractions. MS was used to confirm the identity of the delivere d radiolabelled test item and of metabolites isolat ed from urine. LC- nuclear-magnetic resonance (NMR)-MS spec troscopy was also performed on some extracts.

Findings :

Approximately 90% of the administrated dose (AD) wa s eliminated via urine (78.4%), feces (11.6%), milk (0.014%), and edible organs/tissues (0.061%). The h ighest total radioactive residue (TRR) was observed in kidney (0.184 mg-equiv./kg) and liver (0.05 mg-equi v./kg). Significantly lower residues were detected in the muscle: round muscle (0.011 mg-equiv./kg), flank m uscle (0.009 mg-equiv./kg), and loin muscle (0.008 mgequiv./kg); and fat: subcutaneous fat (0.008 mg-equ iv./kg), omental fat (0.003 mg-equiv./kg), and peri renal fat (0.003 mg-equiv./kg). The TRR in milk samples was in the range of 0.0038-0.0261 mg-equiv./kg with in the observation period of 96 hours.

### - 17 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.2.1-1: Total Radioactive Residue (TRR) in Milk [Azaspirodecenyl-3- 14 C] Spirotetramat

Matrix Collection Timing (hrs after 1 st dose) % AD + mg-equiv./kg

0 1 st dose -- --

8 0.0019 0.0113

24 2 nd

dose 0.0009 0.0038

32 0.0024 0.0150

48 3 rd dose 0.0013 0.0053

56 0.0032 0.0261

72 4 th dose 0.0012 0.0061

80 0.0022 0.0140 Milk

96 0.0009 0.0039



### The parent compound was not detected in samples of milk, muscle, fat, liver and kidney. The major metabolites detected were BYI 08330-enol (33.7-78.4 % of the TRR) and BYI 08330-enol-glucuronide (14.2- 37.4% of the TRR). Three other minor metabolites ( BYI 08330-ketohydroxy, BYI 08330-desmethyl-enol, an d BYI 08330-mono-hydroxy) were found each at less tha n 10% of the TRR.

Table B.7.2.1-2: Summary of Characterization/Identi fication of Radioactive Residues in Livestock Matrices Following Application of 14C-Spirotetramat at 2.2 mg/kg bw for 4 consecutive days. Muscle Fat Liver Kidney Milk (day 4 pool)TRRs = 0.011 mgequiv./kg TRRs = 0.003

mg-equiv./kg TRRs = 0.050 mgequiv./kg TRRs = 0.184

mg-equiv./kg TRRs = 0.008

mg-equiv./kg Compound

% TRR mgequiv./ kg % TRR mgequi v./kg % TRR mgequiv./ kg % TRR mgequi v./kg %TRR mgequiv. /kg

Parent Spirotetramat -- -- -- -- -- -- -- -- -- --

BYI 08330-enol-GA -- -- 19.4 0.00 1 37.4 0.019 14.2 0.02 6 23.9 0.002

BYI 08330- desmethyl-enol 7.4 0.001 -- -- 6.6 0.003 4.4 0.00 8 7.9 0.001

BYI 08330-monohydroxy -- -- -- -- 4.1 0.002 -- -- 2.3 <0.00 1 BYI 08330-enol 72.4 0.008 59.9 0.00 2 33.7 0.017 78.4 0.14 4 48.8 0.004

BYI 08330- ketohydroxy 9.7 0.001 -- -- 2.7 0.001 2.1 0.00 4 2.3 <0.00

1 Unknown -- -- -- -- 10.7 0.005 0.9 0.00 2 14.9 0.001

Total identified 89.6 0.010 79.3 0.00 2 84.3 0.042 99.1 0.18 2 85.1 0.007

Total characterized -- -- -- -- 10.7 0.005 0.9 0.00 2 14.9 0.001

Total extractable 89.6 0.10 79.3 0.00 2 95.0 0.047 100 0.18 4 100 0.008

Unextractable - PES 1 -- -- 20.7 0.00 1 4.7 0.002 -- -- -- --

Accountability 2 100 0.011 100 0.00 3 100 0.05 100 0.18 4 100 0.008

1 Residues remaining after extractions. 2 Accountability = (Total extractable + Total unextr actable)/(TRRs from combustion analysis).

### - 18 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Conclusion : The metabolism of spirotetramat in ruminants involv ed cleavage of the ester group to the primary metab olite BYI 08330-enol followed by conjugation of the enol hydroxy group with glucuronic acid to BYI 08330-eno lGA. Oxidation of the azaspirodecenyl moiety to BYI 08330-ketohydroxy and demethylation of the methoxy group to BYI 08330-desmethyl-enol were minor metabo lic reactions as well as reduction of the azaspirodecenyl moiety to BYI 08330-monohydroxy.

B.7.2.2 Metabolism in laying hen

Reference: Metabolism of [Azaspirodecenyl-3-14C] BYI 08330 in the Laying Hen Author(s), year: Koester, J., Klempner, A., 2006 Report/Doc. number: Report No.: MEF-05/273, Edition Number: M-268574-01-2 Guideline(s): PMRA Directive 98-02; DACO 6.2/EPA OP PTS 860.1300 GLP: Yes. Deviations: No. Validity: Yes.

Materials and method :

The nature of the residue in eggs and tissues was i nvestigated with 6 laying hens dosed orally once da ily by gavage with [azaspirodecenyl-3- 14 

### C]spirotetramat at a rate of 1.01 mg a.i./kg bw/day (12.86 mg/kg in feed) for 14 days. Eggs and excreta were collected daily . The treated hens were sacrificed ca. 24 hrs afte r the last dosage. Liver, kidney, muscle (leg, breast), fat (subcutaneous), skin (without fat) were collect ed.

Tissues (except fat) were homogenized in half-froze n state using a mincing machine. An aliquot of eac h resulting tissue pulp was weighed, freeze-dried, we ighed again, homogenized and determined triply for radioactivity by combustion following LSC. Aliquot s of subcutaneous fat and skin without fat were wei ghed and solubilized with BTS-450 and measured for radio activity by LSC. Gall bladders were punctured for the collection of the bile fluid.

Aliquot samples from egg pool, combined muscle, sub cutaneous fat, liver and excreta samples were used for metabolite analysis. Each tissue type was extr acted 3-4 times with ACN water. The extracts of ea ch sample were combined and cleaned-up using reverse-p hase SPE. Flow through fractions and rinse solutio n of each sample were combined and concentrated prior to HPLC analysis.

Metabolite identification was carried out via HPLC co-chromatography with reference standards. Normal

phase thin-layer chromatography (TLC) co-chromatogr aphy was applied as a second method. Individual peak fractions were subsequently analyzed by TLC co -chromatography together with the respective reference items. MS was used to confirm the identi ty of the delivered radiolabelled test item. LC- nu clearmagnetic resonance (NMR)-MS spectroscopy was also p erformed on some extracts.

Findings :

The majority of the radioactivity (90% of the admin istered dose, AD) was detected in the excreta. Onl y 0.045% and 0.023% of the total AD were detected in the eggs and edible organs/tissues, respectively. The highest total radioactive residue (TRR) was detecte d in kidneys (0.039 mg-equiv./kg) and liver (0.017 mgequiv./kg), followed by fat (0.004 mg-equiv./kg), a nd muscle (0.003 mg-equiv./kg). The average TRR in eggs was 0.015 mg-equiv./kg.

### - 19 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

The parent compound was not detected in any of the samples. BYI 08330-enol was the major metabolite detected in eggs, liver, fat and muscle (18-84% of the TRR; 0.001-0.013 mg-equiv./kg). The glucuronic acid conjugate BYI 08330-enol-GA was also detected in eg gs (6.9% of the TRR, 0.001 mg-equiv./kg), muscle (4.2% of the TRR, <0.001 mg-equiv./kg) and liver (1 5.1% of the TRR, 0.003 mg-equiv./kg).

Table B.7.2.2-1: Summary of Characterization and Id entification of Radioactive Residues in Livestock Matrices Following Application of Radiolabelled Spi rotetramat at 1.01mg/kg bw for 14 Consecutive Days. Muscle Fat Liver EggsTRRs = 0.003 mgequiv./kg TRRs = 0.004 mgequiv./kg TRRs = 0.017 mgequiv./kg TRRs = 0.015 mgequiv./kg Compound

% TRR mgequiv./k g % TRR mgequiv./kg % TRR mgequiv./kg %TRR mgequiv./kg

Spirotetramat -- -- -- -- -- -- -- -- BYI 08330-enol-GA 4.2 <0.001 -- -- 15.1 0.003 6.9 0. 001 Unknown 1 6.9 <0.001 -- -- 3.6 0.001 4.7 0.001

BYI 08330-enol 64.4 0.002 18.4 0.001 50.0 0.009 83.9 0.013

Unknown 2 A -- -- 56.5 0.002 -- -- -- -- Total identified 68.6 0.002 18.4 0.001 65.1 0.011 9 0.8 0.014 Total characterized 6.9 <0.001 56.5 0.002 3.6 0.001 4.7 0.001 Total extractable 75.6 0.002 74.9 0.003 68.6 0.012 95.5 0.014 Unextractable (PES) 1 24.4 0.001 25.1 0.001 30.0 0.005 4.5 0.001 Accountability 2 100 0.003 100 0.004 98.6 0.017 100 0.015 1 Residues remaining after extractions. 2 Accountability = (Total extractable + Total unextr actable)/(TRRs from combustion analysis). A Presumably fatty acid conjugate of BYI 08330-enol or related metabolite.



### Conclusion :

Laying hens metabolized spirotetramat intensively a nd no parent compound was detected in any sample. Spirotetramat was mainly metabolized in laying hens by: 1) Cleavage of the ester bond of the side chai n yielding BYI 08330-enol. 2) Conjugation of BYI 083 30-enol with glucuronic acid. 3) Demethylation of the cyclohexyl- O -methyl group to the respective alcohol and 4) hydr oxylation in the pyrrolidine ring of BYI 08330- enol resulting in BYI 08330-ketohydroxy.

Comments (RMS):

B.7.2.3 Overall conclusion on the metabolic fate in livestock animals:

The submitted goat and poultry metabolism data are adequate to satisfy data requirements. The biodegradation of spirotetramat in livestock can be characterized as cleavage of the carbonate ester g roup to the primary metabolite BYI 08330-enol followed by c onjugation of the enol hydroxy group with glucuroni c acid to BYI 08330-enol-GA. Oxidation of the azaspi rodecenyl moiety to BYI 08330-ketohydroxy and demethylation of the methoxy group to BYI 08330-des methyl-enol were minor metabolic reactions in ruminants as well as reduction of the azaspirodecen yl moiety to BYI 08330-monohydroxy. Based on the currently proposed uses, the residue definition for the expression of the MRL in livestock commodities is spirotetramat and the metabolite BYI 08330-enol. Th e residue definition for dietary exposure assessmen t in livestock commodities is spirotetramat and the meta bolites BYI 08330-enol and BYI 08330-enol-GA.

### - 20 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Figure B.7.2.3-1: Proposed metabolic pathway of spi rotetramat in livestock:

BYI 08330 (parent)

BYI 08330-enol

BYI-08330- ketohydroxy BYI-08330- desmethyl-enol BYI 08330- mono-hydroxy (lactating goats only) Congugation with glucuronic acid



### Chemical Names and Structures of Spirotetramat and Metabolites.

Common name/code Chemical name Chemical structure Spirotetramat (parent) cis -3-(2,5-dimethylphenyl)-8- methoxy-2-oxo-1-azaspiro [4.5]dec-3-en-4-yl ethyl carbonate

BYI 08330-ketohydroxy cis -3-(2,5-dimethylphenyl)-3- hydroxy-8-methoxy-1- azaspiro [4.5]decane-2,4- dione

### - 21 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

BYI 08330-enol cis -3-(2,5-dimethylphenyl)-4- hydroxy-8-methoxy-1- azaspiro [4.5]dec-3-en-2-one

BYI 08330-enol-alcohol cis -4-hydroxy-3-[5- (hydroxymethyl)-2- methylphenyl]-8-methoxy-1-azaspiro[4.5]dec3-en-2-one

BYI 08330-monohydroxy cis -3-(2,5-dimethylphenyl)-4-hydroxy-8-methoxy1-azaspiro[4.5]decan-2-one

BYI 08330-desmethylketohydroxy cis -3-(2,5-dimethylphenyl)- 3,8-dihydroxy-1-azaspiro[4.5] decane-2,4-dione

BYI 08330-di-hydroxy cis -3-(2,5-dimethylphenyl)- 3,4-dihydroxy-8-methoxy-1- azaspiro[4.5]decan-2-one

### - 22 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

BYI 08330-desmethylketohydroxy-glucoside (isomers), in leaves also +BYI 08330-ketohydroxy-formiateglycoside (Isomers) cis -3-(2,5-dimethylphenyl)-8- hydroxy-2,4-dioxo-1- azaspiro[4.5]dec-3-yl hexopyranoside cis-3-(2,5-dimethylphenyl)-3- hydroxy-2,4-dioxo-1- azaspiro[4.5]dec-8-yl hexopyranoside

+ cis -3-(2,5-dimethylphenyl)-3- (hexopyranosyloxy)-2,4- dioxo-1-azaspiro [4.5]dec-8- yl formate +



### BYI 08330-enol-Glc cis -3-(2,5-dimethylphenyl)-8- methoxy-2-oxo-1-azaspiro[4.5]dec-3-en-4-yl beta-Dglucopyranoside

BYI 08330-enol-GA glucuronic acid conjugate of cis -3-(2,5-dimethylphenyl)-4-hydroxy-8-methoxy1-azaspiro[4.5]dec-3-en-2-one

BYI 08330-desmethylenol OrBYI 08330-4-hydroxyenol cis -3-(2,5-dimethylphenyl)- 4,8-dihydroxy-1-azaspiro[4.5]dec3-en-2-one

BYI 08330-desmethylenol-Glc Glucoside of cis -3-(2,5- dimethylphenyl)- 4,8-dihydroxy-1-azaspiro[4.5]dec3-en-2-one

### - 23 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

BYI 08330-MA-amide Cis -1-{[(2,5-dimethylphenyl) (hydroxy)acetyl]amino}-4- methoxycyclohexanecarboxylic acid

BYI 08330-mandelic acid amide 2-(2,5-dimethylphenyl)-2- hydroxyacetamide

BYI 08330-mandelic acid (2,5-dimethylphenyl)(hydroxy) acetic acid

BYI 08330- hydroxymorpholinedion Cis -3-(2,5-dimethylphenyl)-3-hydroxy-9-methoxy-4-oxa1-azaspiro[5.5]undecane-2,5- dione

BYI 08330-olefine 2-(2,5-dimethylphenyl)-2- hydroxy-N-(4- methoxycyclohex-1-en-1- yl)acetamide

or

2-(2,5-dimethylphenyl)-2- hydroxy-N-(4- methoxycyclohexylidene) acetamide

BYI 08330- ketohydroxy-alcohol cis -3-hydroxy-3-[5- (hydroxymethyl)-2- methylphenyl]-8- methoxy-1-azaspiro [4.5]decane-2,4-dione

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

BYI 08330-ketohydroxy-alcoholglycoside glycoside of cis -3-hydroxy3-[5-(hydroxymethyl)-2- methylphenyl]-8- methoxy-1-azaspiro [4.5]decane-2,4-dione

BYI 08330-desmethyldi-hydroxy (5s,8s)-3-(2,5-dimethylphenyl)- 3,4,8-trihydroxy-1- azaspiro[4.5]decan-2-one

BYI 08330-desmethyldihydroxy-Glc-MA glucosyl-malonic acid conjugate of (5s,8s)-3-(2,5- dimethylphenyl)-3,4,8- trihydroxy-1- azaspiro[4.5]decan-2-one

BYI 08330-desmethylenol -alcohol (5s,8s)-4,8-dihydroxy-3-[5- (hydroxymethyl)-2- methylphenyl]- 1-azaspiro[4.5]dec-3-en-2-one

BYI 08330-desmethylketohydroxy-Glc-MA

(isomer 1 & isomer 2) glucosyl-malonic acid conjugate of (5s,8s)-3-(2,5-dimethylphenyl)-3,8-dihydroxy1-azaspiro[4.5]decane-2,4- dione

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

B.7.3 Definition of the residue (Annex IIA 6.7; Ann ex IIIA 8.7)

The nature of the residue in plants, rotational cro ps, and livestock is adequately understood based on acceptable metabolism studies conducted on apple, l ettuce, cotton, potato, rotational crops, lactating goats, and laying hens.

The residue definition for the expression of the MR L/monitoring and dietary exposure assessment for plant commodities is spirotetramat and the metabolites BYI 08330-eno l, BYI 08330-ketohydroxy, BYI08330-enolGlc, and BYI 08330-mono-hydroxy.

The metabolism of spirotetramat in rotational crops appears to be consistent with the pathway observed in the plant metabolism studies. The following potential components of the residue definition were identifi ed in the confined rotational crop study: BYI08330, BYI08330-ketohydroxy, and free and conjugated BYI08330-desmethyl-ketohydroxy, BYI08330-desmethyl-di-hydroxy and BYI-08330-ketohyd roxy-alcohol. None of these residues were found in the limited rotational crop field trials at a 30-da y PBI. The expected residues in rotational crops are covered sufficiently by the residue definition for the expr ession of the MRL/monitoring and risk assessment fo r plant commodities (spirotetramat and the metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI08330-enolGlc, and BYI 08330-mono-hydroxy), based on the outc ome of the field trials in succeeding crops, which are accepted by RMS Austria as additional information.

Based on the currently proposed uses, the residue d efinition for the expression of the MRL/monitoring for livestock commodities is spirotetramat and the metabolite BYI 08330-enol and the residue definition for the dietary exposure assessment for livestock commodities is spirotetramat and the metabolites BYI 08330-enol and BYI 08330-enol-GA. Comment by RMS AT: The BYI 08330 metabolism studies in ruminants and p oultry were similar in that the majority of BYI 083 30 was metabolized to BYI 08330-enol. Based on the pre dominant residue, the residue definition for monito ring in animal matrices is the parent spirotetramat (BYI 08330) and the metabolite BYI 08330-enol, expresse d as spirotetramat (BYI 08330). Another major metabolite detected in ruminants (up to 24% TRR in milk; see table B.7.2.1-1) and in pou ltry (up to 7% in eggs; see table B.7.2.1-2) was the BYI 08330-enol glucuronic conjugate, therefore this metabolite was also included in the residue definit ion for risk assessment. Considering that the residue definitions for enforc ement and for the riskassessment are different, the conversion factors could be proposed for the riskas sessment based on the metabolism studies. Livestock feeding studies in lactating cows were performed ac cording to the residue definition for riskassessmen t and resulted in average residues of spirotetramat equiv alents less than the LOQ (0.01 mg/kg) in fat, muscl e and liver at the 3-mg/kg dosing level (expected dietary burden: 1.9 mg a.i./kg feed calculated on dry weig ht basis). Only in kidney, residues of 0.022 mg/kg wer e found resulting in a tissue burden in kidney of 0 .014 mg/kg. Total spirotetramat residue in the milk samp les from the 30-mg/kg feeding level were at or belo w the LOQ (0.005 mg/kg) with the exception of a maximum r esidue of 0.006 mg/kg in one cow on study day 10. Residues of parent equivalents did not concentrate in samples of skim milk or milk fat separated from whole

milk. Regarding the low-to-zero residue situation in food of animal origin, it is not considered necessary t o propose conversion factors.

B.7.4 Use pattern for European Trials

Spirotetramat (BYI 08330) is an effective insectici de against aphids, scales, mealy bugs, psyllids, wh ite flies and selected thrips. It acts mainly against immatur e stages and requires oral ingestion.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Spirotetramat is highly systemic and possesses not only xylem-, but also phloem-mobility. Once taken u p by the plant, the active substance moves acropetal in the xylem and acropetal and basipetal in the phloem

. After treatment, even the new shoots or the roots a re protected from sap-sucking pests due to this spe cific biological property. Spirotetramat is intended to be used as an insectic ide in agriculture on a range of crops such as citr us, pome and stone fruits; tree nuts, grape; strawberries, f ruiting and leafy vegetables (indoor and outdoor); brassica vegetables, hops but also on tubers vegetables and tropical fruits such as pineapple, mangoes, bananas and cotton. It is also considered, to use the product o n ornamentals and trees.- 27 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008B.7.5 Intended uses of spirotetramat i.e. supporteduses for evaluation under Directive 91/414/EEC andfor NAFTATable B.7.5-1: The supported European use patternof spirotetramat for Annex I – inclusion, and theintended European use pattern for MRL-setting(marked grey):Crop and/or situationCountryFGorIPests orGroup ofpestscontrolledFormulation ApplicationApplication rate pertreatmentPHI Remarks:(a) (b) (c)Type(d-f)Conc.of as(i)methodkind(f-h)growthstage &season(j)numberminmax(k)intervalbetweenappl.(min)kgas/hLminmaxwaterL/haminmaxkgas/haminmax(days)(l)(m)Citrusall typesEU-S F scales,aphids,mealy bugs,mitesOD 150 spray BBCH 78at lastapplication2 21 0.00961000L/haand mCH*,max3000L/ha0.096kgas./haand mCH*,max0.288kgas./ha(3metres)14 representativeuse for the EUevaluationLettucehead andleafyEU-NEU-SF aphids OD 150 spray BBCH 48at lastapplicationmax. 2 14 0.0072 -0.0144500-10000.072 7 representativeuse for the EUevaluationLettuce,head andleafyEU-NEU-SG aphids OD 150 spray BBCH 48at lastapplicationmax. 2 14 0.0072 -0.0144500-10000.072 7 representativeuse for the EUevaluationpome fruitsapple/pearsEU-NEU-SFaphids,scales,mitesPsylla pyriSC240& MerosprayBBCH 81at lastapplication2140.0144500L/haand mCH*,max1500L/ha0.072kg as/ha andm CH*,max0.216kg as/ha21all applicationdata refer tometre CH*(canopy height,max. heightreferred to isthree (3) metres- 28 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Crop and/or situationCountryFGorIPests orGroup ofpestscontrolledFormulation ApplicationApplication rate pertreatmentPHI Remarks:(a) (b) (c)Type(d-f)Conc.of as(i)methodkind(f-h)growthstage &season(j)numberminmax(k)intervalbetweenappl.(min)kgas/hLminmaxwaterL/haminmaxkgas/haminmax(days)(l)(m)stone fruitplumsour andsweet cherrypeach,apricot,nectarineEU-NEU-SFaphids,scales,mitesSC240& MerosprayBBCH 81at lastapplication2140.0144500L/haand mCH*max1500L/ha0.072kg as/ha andm CH*,max0.216kgas./ha21all applicationdata refer tometre CH*(canopy height,max. heightreferred to isthree (3) metresGrapesEU-NFmealybug,phylloxeraOD150sprayBBCH 822140.0048-0.00721000-15000.07214GrapesEU-SFmealybugphylloxeraOD150sprayBBCH 822140.0048-0.00721000-15000.09614StrawberriesEU-NEU-SFaphids,whitefliesOD150sprayBBCH 872140.0096-0.0192500-10000.0963StrawberriesEU-NEU-SGaphidswhitefliesOD150sprayBBCH 872140.0096-0.0192500-10000.0963OnionsEU-NFThripstabaciOD150sprayBBCH 45470.009-0.012600-8000.0727fruitingvegetablestomatoes,peppers,auberginesEU-SFaphids,whiteflies,mitesOD150sprayBBCH 87at lastapplicationmax 470.0072-0.0096750-10000.0723fruitingvegetablestomatoes,peppers,auberginesEU-NEU-SGaphids,whiteflies,mitesOD150sprayBBCH 87at lastapplicationmax 470.0096750L/haandmetreCH*,max.1500L/ha0.072kg as/haandmetreCH*,max.0.144kg as/ha3all applicationdata refers tometre CH*(canopy height),as fruitingvegetables ingreenhousesmay grow up totwo (2) metres- 29 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Crop and/or situationCountryFGorIPests orGroup ofpestscontrolledFormulation ApplicationApplication rate pertreatmentPHI Remarks:(a) (b) (c)Type(d-f)Conc.of as(i)methodkind(f-h)growthstage &season(j)numberminmax(k)intervalbetweenappl.(min)kgas/hLminmaxwaterL/haminmaxkgas/haminmax(days)(l)(m)Cucurbitvegetablescucumbers,courgettes,melon,watermelonEU-SFaphids,whiteflies,mitesOD150sprayBBCH 87at lastapplicationmax 470.00967500.0723Cucurbitvegetablescucumbers,courgettes,EU-NEU-SGaphids,whiteflies,mitesOD150sprayBBCH 87at lastapplicationmax 470.0096750L/haand mCH*,max1500L/ha0.072kg as/haand mCH*,max0.144kg as/ha3all applicationdata refers tometre CH*(canopy height,as cucumbers ingreenhousesmay grow up totwo (2) metresMelon,watermelonEU-NEU-SGaphids,whiteflies,mitesOD150sprayBBCH 87at lastapplicationmax 470.00967500.0723Floweringbrassica(cauliflower,broccoli),headcabbage(red, whiteSavoy)EU-NEU-SFaphidsOD150sprayBBCH 79at lastapplicationmax 2140.0072–0.0144500-10000.0723Brusselssprouts,kohlrabiEU-NFaphidsOD150sprayBBCH 79at lastapplicationmax 2140.0072–0.0144500-10000.0723LeafybrassicaEU-NEU-SFaphidsOD150sprayBBCH 79at lastapplicationmax 3140.0072–0.0144500-10000.0723- 30 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Crop and/or situationCountryFGorIPests orGroup ofpestscontrolledFormulation ApplicationApplication rate pertreatmentPHI Remarks:(a) (b) (c)Type(d-f)Conc.of as(i)methodkind(f-h)growthstage &season(j)numberminmax(k)intervalbetweenappl.(min)kgas/hLminmaxwaterL/haminmaxkgas/haminmax(days)(l)(m)Beans,greenEU-NEU-SGaphids,whiteflies,mitesOD150sprayBBCH 87470.0048-0.0096750L/haand mCH*,max1500L/ha0.072kg as/haand mCH*,max144 kgas/ha14max. 2 metres ofplant heightHopsEU-NFaphids,scales,mitesOD150sprayBBCH 751n.a.0.007 -0.00452200 -3300-0.15014* CH: Canopy HeightTable B.7.5-2: Summary of representative uses evaluated (spirotetramat), and the intended American usepattern for MRL:Crop and/or situationMemberStateorCountryFGorIPests orGroup ofpestscontrolledPreparationApplicationApplication rate per treatment(for explanation see the textin front of this section)PHI(days)Remarks(a)(b)(c)Type(d-f)Conc.of as(i)methodkind(f-h)growthstage &season(j)numbermin/max(k)intervalbetweenapplications (min)kgas/hLmin –max(l)waterL/hamin –maxkg as/hamin –max(l)(m)Citrusall typesUSA F Scales,aphids,mealy bugs,mites,leafminer,whiteflies,citruspsyllidODSC150240Spray 1-3 21 0.088 –0.1761 Max. dose perseason is 0.351kg/ha- 31 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008PomeFruitsApples/pears/quinces/etc.USA/CanadaF Aphids,scales,mites,mealy bugs,Psylla pyriODSC150240spray 1-3 14 0.088 –0.1547 Max. dose perseason is 0.439kg/haStone fruitPlum, sourand sweetcherry,peach,apricot,nectarine,etc.USA/CanadaF Aphids,scales,mites,mealy bugsODSC150240spray 1-3 14 0.088 –0.1547 Max. dose perseason is 0.263kg/haTree nutsAll typesUSA/CanadaF Aphids,scales,mealy bugs,phylloxeraODSC150240spray 1-3 14 0.088 –0.1547 Max. dose perseason is 0.373kg/haFruitingvegetablesTomatoes,peppers,eggplant,chili,groundcherryUSACanadaF Aphids,whiteflies,psyllids,mitesODSC150240spray 1-3 7 0.055 –0.0881 Max. dose perseason is 0.176kg/haCucurbitvegetablesUSACanadaF Aphids,whiteflies,spider mitesODSC150240spray 1-3 7 0.055 –0.0881 Max. dose perseason is 0.176kg/ha- 32 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008LeafyvegetablesBrassicas(all types)and nonbrassicas(spinach,celery,endive,fennel,head andleaf lettuce,arugula,parsley,cress,radicchio,Swisschard,rhubarbUSACanadaF Aphids,whiteflies,diamondback mothODSC150240spray 1-3 7 0.055 –0.088Brassicacrops:1Leafy,nonbrassicacrops:3Max. dose perseason is 0.176kg/hahops USA F Aphids,mitesODSC150240spray 1 - 2 14 0.088 –0.1107 Max. dose perseason is 0.219grapes USACanadaF Mealy bugs,phylloxera,mites,scalesODSC150240spray 1 - 2 30 0.088 –0.1327 Max. dose perseason is 0.219kg/ha- 33 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008TubervegetablesArracacha,arrowroot,artichokes,canna,cassava,chayote,chufa,dasheen,ginger,leren,potato,sweetpotato,tanier,tumeric,yamUSACanadaF Aphids,psyllids,whiteflies,mites,potatotubewormODSC150240spray 1 - 2 7 0.066 –0.0887 Max. dose perseason is 0.176kg/ha∗For uses where the column "Remarks" is marked in grey further consideration is necessary.Uses should be crossed out when the notifier no longer supports this use(s).** The rate range listed is the lowest and highestrate approved for use on a crop group. Specific ratesfor a pest(s) may vary(a) For crops, the EU and Codex classifications (both) should be taken into account; whererelevant, the use situation should be described (e.g. fumigation of a structure)(b) Outdoor or field use (F), greenhouse application (G) or indoor application (I)(c)e.g.biting and suckling insects, soil born insects, foliar fungi, weeds(d)e.g.wettable powder (WP), emulsifiable concentrate (EC), granule (GR)(e) GCPF Codes - GIFAP Technical Monograph No 2, 1989(f) All abbreviations used must be explained(g) Method, e.g. high volume spraying, low volume spraying, spreading, dusting, drench(h) Kind,e.g.overall, broadcast, aerial spraying, row, individual plant, between the plant- typeof equipment used must be indicated(i) g/kg or g/L. Normally the rate should be givenfor the active substance (according toISO) and not for the variant in order to compare the rate for same active substances used indifferent variants (e.g. fluoroxypyr).(j) Growth stage at last treatment (BBCH Monograph,Growth Stages of Plants, 1997,Blackwell, ISBN 3-8263-3152-4), including where relevant, information on season at time ofapplication(k) Indicate the minimum and maximum number of application possible under practicalconditions of use(l) The values should be given in g or kg whatevergives the more manageable number(e.g. 200 kg/ha instead of 200 000 g/ha or 12.5 g/ha instead of 0.0125 kg/ha(m) PHI - minimum pre-harvest interval- 34 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Table B.7.5-3: Summary of the representative uses evaluated (spirotetramat), and the intended Canadianuse pattern for MRL:Crop and/orsituationMemberStateorCountryFGorIPests orGroup ofpestscontrolledPreparationApplicationApplication rate pertreatment**(for explanation see the textin front of this section)PHI(days)Remarks(a)(b)(c)Type(d-f)Conc.of as(i)methodkind(f-h)growthstage &season(j)numbermin/max(k)intervalbetweenapplications (min)kgas/hLmin –max(l)waterL/hamin –maxkgas/hamin –max(l)(m)Citrusall typesUSA F Scales,aphids,mealy bugs,mites,leafminer,whiteflies,citruspsyllidODSC150240Spray 1-3 21 0.088 –0.1761 Max. dose perseason is 0.351kg/haPomeFruitsApples/pears/quinces/etc.Canada F Rosy appleaphid, appleaphids, SanJose scale,mealybugs,pear psylla,whitefliesODSC150240spray 1-5 14 0.088 –0.1407 Max. dose perseason is 0.440kg/haStone fruitPlum, sourand sweetcherry,peach,apricot,nectarine,etc.Canada F Aphids,Whitelfies,San Josescale,Whitepeachscale,Lecaniumscale,mealy bugsODSC150240spray 1-3 14 0.088 –0.1407 Max. dose perseason is 0.270kg/ha- 35 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Crop and/orsituationMemberStateorCountryFGorIPests orGroup ofpestscontrolledPreparationApplicationApplication rate pertreatment**(for explanation see the textin front of this section)PHI(days)Remarks(a)(b)(c)Type(d-f)Conc.of as(i)methodkind(f-h)growthstage &season(j)numbermin/max(k)intervalbetweenapplications (min)kgas/hLmin –max(l)waterL/hamin –maxkgas/hamin –max(l)(m)Tree nutsAll typesCanada F Aphids,Whiteflies,San Josescale,Walnutscale,Lecaniumscale,mealy bugs,phylloxeraODSC150240spray 1-4 14 0.088 –0.1407 Max. dose perseason is0.380kg/haFruitingvegetablesTomatoes,peppers,eggplant,chili,groundcherryCanada F Aphids,whiteflies,psyllids,ODSC150240spray 1-3 7 0.052 –0.0881 Max. dose perseason is 0.175kg/haCucurbitvegetablesCanada F Aphids,whiteflies,ODSC150240spray 1-3 7 0.052 –0.0881 Max. dose perseason is 0.176kg/ha- 36 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Crop and/orsituationMemberStateorCountryFGorIPests orGroup ofpestscontrolledPreparationApplicationApplication rate pertreatment**(for explanation see the textin front of this section)PHI(days)Remarks(a)(b)(c)Type(d-f)Conc.of as(i)methodkind(f-h)growthstage &season(j)numbermin/max(k)intervalbetweenapplications (min)kgas/hLmin –max(l)waterL/hamin –maxkgas/hamin –max(l)(m)LeafyvegetablesBrassicas(all types)and nonbrassicas(spinach,celery,endive,fennel,head andleaf lettuce,arugula,parsley,cress,radicchio,Swisschard,rhubarbCanada F Aphids,whiteflies,ODSC150240spray 1-3 7 0.052 –0.088Brassicacrops:1Leafy,nonbrassicacrops:3Max. dose perseason is 0.175kg/hahops Canada F Hop aphid ODSC150240spray 1 - 2 14 0.088 –0.1057 Max. dose perseason is 0.220Grapes andsmall fruitvineclimbing(exceptkiwifruit)Canada F Mealy bugs,phylloxera,whiteflies,LecaniumscaleODSC150240spray 1 - 2 30 0.088 –0.1407 Max. dose perseason is0.220kg/ha- 37 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Crop and/orsituationMemberStateorCountryFGorIPests orGroup ofpestscontrolledPreparationApplicationApplication rate pertreatment**(for explanation see the textin front of this section)PHI(days)Remarks(a)(b)(c)Type(d-f)Conc.of as(i)methodkind(f-h)growthstage &season(j)numbermin/max(k)intervalbetweenapplications (min)kgas/hLmin –max(l)waterL/hamin –maxkgas/hamin –max(l)(m)TubervegetablesArracacha,arrowroot,artichokes,canna,cassava,chayote,chufa,dasheen,ginger,leren,potato,sweetpotato,tanier,tumeric,yamCanada F Aphids,psyllids,whiteflies,ODSC150240spray 1 - 2 7 0.052 –0.0887 Max. dose perseason is 0.175kg/ha∗For uses where the column "Remarks" is marked in grey further consideration is necessary.Uses should be crossed out when the notifier no longer supports this use(s).** The rate range listed is the lowest and highestrate approved for use on a crop group. Specific ratesfor a pest(s) may vary(a) For crops, the EU and Codex classifications (both) should be taken into account; whererelevant, the use situation should be described (e.g. fumigation of a structure)(b) Outdoor or field use (F), greenhouse application (G) or indoor application (I)(c)e.g.biting and suckling insects, soil born insects, foliar fungi, weeds(d)e.g.wettable powder (WP), emulsifiable concentrate (EC), granule (GR)(e) GCPF Codes - GIFAP Technical Monograph No 2, 1989(f) All abbreviations used must be explained(g) Method, e.g. high volume spraying, low volume spraying, spreading, dusting, drench(h) Kind,e.g.overall, broadcast, aerial spraying, row, individual plant, between the plant- type ofequipment used must be indicated(i) g/kg or g/L. Normally the rate should be givenfor the active substance (according toISO) and not for the variant in order to compare the rate for same active substances used indifferent variants (e.g. fluoroxypyr).(j) Growth stage at last treatment (BBCH Monograph,Growth Stages of Plants, 1997,Blackwell, ISBN 3-8263-3152-4), including where relevant, information on season at time ofapplication(k) Indicate the minimum and maximum number of application possible under practicalconditions of use(l) The values should be given in g or kg whatevergives the more manageable number(e.g. 200 kg/ha instead of 200 000 g/ha or 12.5 g/ha instead of 0.0125 kg/ha(m) PHI - minimum pre-harvest interval

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

B.7.6 Residues resulting from supervised trials (An nex IIA 6.3; Annex IIIA 8.3)

Relevant for PMRA (Canada) and USEPA: Summary information of the residue trials conducted in the NAFTA regions can be found in Annex II of t his document.

Relevant for EU: Results from supervised residue trials in lettuce a nd citrus are reported representing the designated intended uses of this Annex II dossier for Annex I inclusion of spirotetramat (BYI08330). In addition, residue data from uses of spirotetrama t in pome fruit, stone fruit, grapes, strawberries, onions, fruiting vegetables, brassica vegetables and hops a re reported and evaluated in order to accelerate th e fixing of MRLs with respect to Regulation 396/2005/EC. Thu s, all possible MRLs are “peer-reviewed” and there is no need for additional work load after Annex I – in clusion for spirotetramat (approach supported by EF SA). Spirotetramat is applied as a spray solution to the different crops. Different formulations of spirote tramat were used: In 2004, residue trials were conducted w ith the OD 100 formulation of BYI08330. Due to a mi nor change of the final formulation from OD 100 to OD 1 50, residue trials in 2005 were conducted with the OD 150 formulation of BYI08330. The composition of bot h formulations is similar; but the amount of the ac tive substance is 100 g as/L in the OD 100 formulation a nd 150 g as/L in the OD 150 formulation. Applied at identical use rates for the active substance, both formulations are considered to be comparable with r espect to residues.

Results from additional residue trials in lettuce, pome fruit and pepper are reported, which were cond ucted using the SC 240 formulation of BYI08330 with the a ddition of 0.2 % RME (rape methyl ester) to the spr ay solution. Moreover 4 residue trials, 2 trials in gr apes and 2 trials in pepper were conducted with the SC 048 formulation of BYI08330. The results of these trial s are reported to give a complete picture of the BY I08330 residue behaviour.

Analysis of residue samples was conducted according to method 00875 (see Chapter IIA 4.3). The single analytes (spirotetramat and its metabolites BYI0833 0-enol, -ketohydroxy, -monohydroxy and -enol-glucos ide) are determined by HPLC-MS/MS. The results are expre ssed as parent equivalents. The total residue of spirotetramat is calculated by summing up the value s determined for the individual analytes expressed as parent equivalent. Expressed as parent equivalents the LOQ is 0.01 mg/kg for spirotetramat, 0.012 mg/k g for BYI08330-enol, -ketohydroxy and –monohydroxy and 0. 08 mg/kg for BYI08330-enol-glucoside. For hop cones the respective LOQs are by a factor of 10 hig her. The LOQ for the calculated total residue of BYI08330 is quoted at 0.054 mg/kg (hops 0.54 mg/kg)

. For each trial residues at the envisage PHI of the critical European GAP were evaluated. If, however, the total residue of spirotetramat at later intervals e xceeded the total residue at the PHI, the higher va lues were evaluated to cover the worst case residue. The resi due data of each trial used for the evaluation are marked in bold in the respective tables which summarise th e residue results.

B.7.6.1 Citrus fruits

Spirotetramat is applied for control of scales, aph ids, mealy bugs and mites in citrus. European resid ue data were submitted in two studies on oranges and two st udies on mandarins to support the use of BYI08330 i n citrus in southern Europe. The critical European GA P is summarized in Table B.7.6.1-1:

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.6.1-1: GAP for residue situation in citru s fruits

Indoor or outdoor Number of

applications North or

South of EU Growth stage at

last application Application rate expressed

under the relevant unit PHI (d) EU-S F 2 Spray BBCH 78 0.096 kg a.s./ha and m canopy height, max. 0.288 kg a.s./ha 14



### Reference: Determination of residues of BYI08330 in/on orange after spraying of BYI08330 (100 OD) in the field in Italy, Portugal a nd Spain, Author(s), year: Schöning R., Helfrich P., 2005 Report/Doc. number: RA-2032/04, including trials no . R 2004 0139/6, R 2004 0141/8, R 2004 0239/2, R 2004 0240/6 M-263546-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: yes Deviations: No Validity: yes

Reference: Determination of residues of BYI08330 in/on orange after spraying of BYI08330 (150 OD) in the field in Portugal, Italy a nd Spain Author(s), year: Schöning R.; Wieland K.; 2006 Report/Doc. number: RA-2003/05, including trials no . R 2005 0046/7, R 2005 0047/5, R 2005 0048/3, R 2005 0049/1 M-269908-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: yes Deviations: No Validity: yes

Reference: Determination of residues of BYI08330 in/on mandari n after spraying of BYI08330 (100 OD) in the field in Italy, Portugal a nd Spain Author(s), year: Schöning R.; Helfrich P.; 2005 Report/Doc. number: RA-2033/04, including trials no . R 2004 0142/6, R 2004 0143/6, R 2004 0237/6, R 2004 0238/4 M-264450-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: yes Deviations: No Validity: yes

### - 40 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Reference: Determination of residues of BYI08330 in/on mandari n after spraying of BYI08330 (150 OD) in the field in Portugal, Spain a nd Italy Author(s), year: Schöning R.; Wieland K.; 2006 Report/Doc. number: RA-2002/05, including trials no . R 2005 0041/6, R 2005 0042/4, R 2005 0043/2, R 2005 0044/0, R 2005 0045/9 M-270179-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: yes

Experimental design: The magnitude of residues of spirotetramat and its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-mono-hydroxy and BYI 08330-enol-Glc in orange s and mandarins (fruit, peel and pulp) harvested following two applications with the formulations BY I 08330 (100 OD, 150 OD) to orange and mandarin tre es in Southern Europe (Italy, Spain and Portugal) was determined. The formulations used were oil based dispersion con centrates containing 100 and 150 g/L spirotetramat. The product was used two times at application rates of 0.096 kg a.s./ha and meter canopy height and a wate r volume of 1000 L per ha and meter canopy height (2 – 3 m), this is corresponding to 0.192 – 0.288 kg a.s./ha. The last applications were carried out at growth stage between BBCH 79 and BBCH 87. Samples were taken before the last application, 0, 7, 14, 2 1 and 28 days after the last application. The distr ibution of the residues in peel and pulp was determined in spe cimens sampled 14, 21 and 28 days after application

. Analytical method used in all studies: Residues of spirotetramat and its metabolites BYI 0 8330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and BYI 08330-enol-Glc were determined by H PLC-ESI-MS/MS according to method 00857. The limit of quantification (LOQ, defined as the lowest validated fortificatio n level) was 0.01 mg/kg for spirotetramat, 0.012 mg/kg for its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and 0.008 mg/kg for BYI 08330-enol-Glc in/o n orange (fruit, peel and pulp), calculated as spirotetramat equivalent. The mean procedural recoveries at the fortification levels of 0.01 to 1.0 mg/kg f or spirotetramat and its four metabolites ranged between 83 and 107 %; these resu lts indicate that the methods used were suitable fo r this analysis. Findings: A detailed summary of the residue trial for citrus fruits is given in Annex Ia. For Southern Europe 8 trials on oranges and 9 trial s on mandarins were submitted according the critica l GAP. The trials were mainly carried out in Italy, S pain and Portugal. All trials were carried out as r esidue decline studies and in addition to the residue resu lts of the whole fruit also the results of peel and pulp were reported. The total residue of spirotetramat ranged between 0.064 and 0.233 mg/kg in orange fruit and between 0.101 and 0.331 mg/kg in mandarin fruit. Co nsidering the whole citrus group the total residue ranged from 0.0645 to 0.331 mg/kg (STMR 0.14 mg/kg)

. In pulp, representing the edible part of citrus, th e total residue ranged from <0.054 mg/kg to 0.146 m g/kg. In citrus peel, the total residue of spirotetramat was between 0.07 and 0.97 mg/kg. Spirotetramat and its enol metabolite were the main metabolites in orange and mandarin fruit, pulp and peel. BYI08330-ketohydroxy and the BYI08330-enol-glucosid e were minor metabolites. BYI08330-monohydroxy was not found.

### - 41 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.6.1-2: Overview of European residue data for spirotetramat and its metabolites in citrus fruits used two times with application rates of 0.096 kg a.s./ha and meter canopy height, corresponding to 0.2112 - 0.288 kg a.s./ha:

crop location portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330- keto hydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 oranges Mineo, Italy,

2004 Fruit

Fruit Fruit Fruit Pulp Peel Fruit Pulp Peel Fruit Pulp Peel 0*

0 7 14 14 14 21 21 21 28 28 28 0.01

0.12 0.03 0.02 <0.01 0.05 0.02 <0.01 0.03 <0.01 <0.01 0.01 0.012

0.012 0.012 0.012 <0.012 0.058 0.012 <0.012 0.037 <0.012 <0.012 0.027 0.012

0.012 0.012 0.012 <0.012 0.030 0.012 <0.012 0.026 <0.012 <0.012 0.024 <0.012

<0.012 <0.012

< 0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 0.008 <0.008 <0.008 0.008 <0.008 <0.008 0.008 <0.054

0.164 0.074 0.064 <0.054 0.158 0.064 <0.054 0.113 <0.054 <0.054 0.081 oranges Catania,

Italy, 2004 Fruit

Fruit Fruit Fruit Pulp Peel Fruit Pulp Peel 0*

0 14 21 21 21 28 28 28 <0.01

0.11 0.02 0.02 <0.01 0.02 0.01 <0.01 0.01 0.012

0.018 0.017 0.014 <0.012 0.059 0.012 <0.012 0.025 0.012

0.012 0.012 0.012 <0.012 0.018 0.012 <0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 0.008 <0.008 <0.008 0.008 <0.054

0.16 0.069 0.066 <0.054 0.117 <0.054 <0.054 0.067 oranges Palmela,

Portugal, 2004 Fruit

Fruit Fruit Fruit Pulp Peel Fruit Pulp Peel Fruit Pulp Peel 0*

0 7 14 14 14 21 21 21 27 27 27 <0.01

0.13 0.13 0.04 <0.01 0.04 0.02 <0.01 0.02 0.01 <0.01 0.01 <0.012

0.023 0.044 0.041 0.015 0.11 0.031 <0.012 0.049 0.033 0.015 0.030 <0.012

<0.012 0.014 0.013 <0.012 0.032 0.013 <0.012 0.026 0.013 <0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 0.008 <0.008 0.008 0.008 <0.008 0.008 0.008 <0.008 0.008 <0.054

0.185 0.208 0.114 0.057 0.202 0.084 <0.054 0.115 0.076 0.057 0.072 oranges Benifaió,

Spain, 2004 Fruit

Fruit Fruit Fruit Pulp Peel Fruit Pulp Peel 0*

0 15 21 21 21 28 28 28 0.07

0.14 0.10 0.08 <0.01 0.14 0.05 <0.01 0.14 0.052

0.062 0.090 0.078 0.063 0.28 0.064 0,056 0.20 <0.012

0.012 0.015 0.012 <0.012 0.035 0.012 <0.012 0.033 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.011

0.012 0.016 0,016 0.008 0.054 0,017 0.008 0.052 0.157

0.238 0.233 0.198 0.105 0.521 0.155 0.098 0.437 oranges Palmela,

Portugal, 2005 Fruit

Fruit Pulp Peel Fruit Pulp Peel Fruit Pulp Peel 0

14 14 14 21 21 21 28 28 28 0.10

0.01 <0.01 0.02 <0.01 <0.01 0.01 0.02 <0.01 0.01 0.020

0.015 <0.012 0.031 <0.012 <0.012 0.032 0.012 <0.012 0.029 0.012

0.012 <0.012 0.016 <0.012 <0.012 0.015 0.012 <0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 0.008 <0.008 <0.008 0.008 0.008 <0.008 0.008 0.152

0.057 <0.054 0.087 <0.054 <0.054 0.077 0.064 <0.054 0.071

### - 42 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop location portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330- keto hydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 oranges Carlentini,

Italy, 2005 Fruit

Fruit Pulp Peel Fruit Pulp Peel Fruit Pulp Peel 0

14 14 14 21 21 21 28 28 28 0.20

0.01 <0.01 0.03 0.02 <0.01 0.05 <0.01 <0.01 0.02 0.013

0.012 <0.012 0.044 0.012 <0.012 0.044 <0.012 <0.012 0.030 0.012

<0.012 <0.012 0.016 0.012 <0.012 0.017 <0.012 <0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 0.008 <0.008 <0.008 0.008 <0.008 <0.008 0.008 0.245

<0.054 <0.054 0.11 0.064 <0.054 0.131 <0.054 <0.054 0.082 oranges Cullera,

Spain, 2005 Fruit

Fruit Fruit Fruit Pulp Peel Fruit Pulp Peel Fruit Pulp Peel 0*

0 7 14 14 14 21 21 21 28 28 28 0.02

0.10 0.06 0.05 <0.01 0.21 0.02 <0.01 0.04 0.01 <0.01 0.01 0.036

0.047 0.049 0.039 0.034 0.20 0.038 0.025 0.098 0.032 0.022 0.072 0.012

0.012 0.024 0.013 <0.012 0.069 0.013 <0.012 0.044 0.012 <0.012 0.027 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.008

0.008 0.008 0.008 0.008 0.023 0.008 0.008 0.016 0.008 0.008 0.014 0.088

0.179 0.153 0.122 0.076 0.514 0.091 0.067 0.21 0.074 0.064 0.135 oranges Catania,

Italy, 2005 Fruit

Fruit Fruit Fruit Pulp Peel Fruit Pulp Peel Fruit Pulp Peel 0*

0 7 14 14 14 21 21 21 28 28 28 0.04

0.11 0.04 0 .03 <0.01 0.06 0.02 <0.01 0.05 0.02 <0.01 0.04 0.012

0.012 0.014 0.015 <0.012 0.090 0.016 <0.012 0.059 0.013 <0.012 0.065 0.013

0.012 0.012 0.012 <0.012 0.042 0.012 <0.012 0.029 0.012 <0.012 0.035 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 0.008 <0.008 <0.008 0.008 <0.008 <0.008 0.008 0.085

0.154 0.086 0.077 <0.054 0.212 0.068 <0.054 0.158 0.065 <0.054 0.16 Mandarin Misterbianc

o, Italy, 2004 Fruit

Fruit Fruit Fruit Pulp Peel Fruit Pulp Peel Fruit Pulp Peel 0*

0 7 14 14 14 21 21 21 28 28 28 0.02

0.21 0.02 0.01 <0.01 0.03 0.02 <0.01 0.03 0.01 <0.01 0.01 0.073

0.13 0.12 0.075 0.045 0.24 0.076 0.053 0.21 0.069 0.035 0.11 0.015

0.023 0.026 0.019 <0.012 0.086 0.023 <0.012 0.080 0.017 <0.012 0.044 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.010

0.012 0.015 0.014 0.008 0.048 0.015 0.008 0.061 0.018 0.008 0.044 0.13

0.387 0.193 0.13 0.087 0.416 0.146 0.095 0.393 0.126 0.077 0.22 Mandarin Chamusca,

Portugal, 2004 Fruit

Pulp Peel Fruit Pulp Peel Fruit Pulp Peel 15

15 15 21 21 21 29 29 29 0.01

<0.01 0.02 0.01 <0.01 0.02 0.01 <0.01 0.02 0.15

0.072 0.21 0.14 0.077 0.18 0.10 0.062 0.13 <0.012

<0.012 0.031 <0.012 <0.012 0.026 <0.012 <0.012 0.016 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.029

0.008 0.075 0.035 0.008 0.081 0.032 0.008 0.073 0.213

0.114 0.348 0.209 0.119 0.319 0.166 0.104 0.251

### - 43 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop location portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330- keto hydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 Mandarin Cullera,

Spain, 2004 Fruit

Fruit Fruit Pulp Peel Fruit Pulp Peel Fruit Pulp Peel 0*

0 14 14 14 21 21 21 29 29 29 0.03

0.20 0.09 <0.01 0.29 0.06 <0.01 0.16 0.03 <0.01 0.07 0.070

0.12 0.15 0.060 0.43 0.13 0.054 0.34 0.12 0.068 0.20 0.019

0.026 0.035 0.012 0.14 0.036 <0.012 0.12 0.026 0.012 0.068 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.020

0.023 0.044 0.011 0.12 0.047 0.011 0.12 0.050 0.015 0.10 0.151

0.381 0.331 0.105 0.992 0.285 0.099 0.752 0.238 0.117 0.45 Mandarin Brenes,

Spain, 2004 Fruit

Fruit Fruit Fruit Pulp Peel Fruit Pulp Peel Fruit Pulp Peel 0*

0 7 15 15 15 21 21 21 28 28 28 0.03

0.19 0.01 0.01 <0.01 0.01 0.01 <0.01 0.01 0.01 <0.01 0.01 0.066

0.098 0.088 0.066 0.045 0.14 0.069 0.034 0.11 0.075 0.022 0.071 0.015

0.016 0.018 0.013 <0.012 0.057 0.012 <0.012 0.052 0.013 <0.012 0.038 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.018

0.016 0.018 0.016 0.008 0.068 0.021 0.008 0.065 0.030 0.008 0.055 0.141

0.332 0.146 0.117 0.087 0.287 0.124 0.076 0.249 0.140 0.064 0.186 Mandarin Palmela,

Portugal, 2005 Fruit

Fruit Pulp Peel Fruit Pulp Peel Fruit Pulp Peel 0

14 14 14 21 21 21 28 28 28 0.18

0.01 <0.01 0.02 0.01 <0.01 0.02 0.01 <0.01 0.03 0.084

0.059 0.032 0.14 0.045 0.029 0.11 0.046 0.032 0.094 0.012

0.012 <0.012 0.026 0.012 <0.012 0.026 0.012 <0.012 0.030 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.008

0.008 <0.008 0.019 0.008 <0.008 0.020 0.008 <0.008 0.026 0.296

0.101 0.074 0.217 0.087 0.071 0.188 0.088 0.074 0.192 Mandarin Alfarp,

Spain, 2005 Fruit

Fruit Pulp Peel Fruit Pulp Peel Fruit Pulp Peel 0

14 14 14 21 21 21 28 28 28 0.11

0.07 0.01 0.23 0.04 <0.01 0.14 0.06 <0.01 0.09 0.078

0.16 0.098 0.57 0.12 0.083 0.30 0.12 0.10 0.33 0.012

0.013 0.012 0.067 0.012 <0.012 0.040 0.014 0.012 0.051 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.008

0.018 0.008 0.064 0.018 0.008 0.055 0.025 0.012 0.085 0.22

0.273 0.14 0.943 0.202 0.125 0.547 0.231 0.146 0.568 Mandarin Vittoria,

Italy, 2005 Fruit

Fruit Pulp Peel Fruit Pulp Peel Fruit Pulp Peel 0

14 14 14 21 21 21 28 28 28 0.15

0.10 <0.01 0.24 0.02 <0.01 0.04 0.02 <0.01 0.04 0.022

0.033 <0.012 0.16 0.031 <0.012 0.10 0.034 <0.012 0.087 0.013

0.032 <0.012 0.11 0.015 <0.012 0.064 0.018 <0.012 0.046 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

0.008 <0.008 0.012 0.008 <0.008 0.015 0.008 <0.008 0.016 0.205

0.185 <0.054 0.534 0.086 <0.054 0.231 0.092 <0.054 0.201

### - 44 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop location portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330- keto hydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 Mandarin Cullera,

Spain, 2005 Fruit

Fruit Fruit Fruit Pulp Peel Fruit Pulp Peel Fruit Pulp Peel 0*

0 7 14 14 14 21 21 21 28 28 28 0.03

0.23 0.14 0.12 <0.01 0.25 0.03 <0.01 0.07 0.01 <0.01 0.03 0.040

0.086 0.092 0.057 0.022 0.22 0.073 0.028 0.18 0.061 0.025 0.13 0.013

0.019 0.042 0.031 0.012 0.12 0.028 0.012 0.10 0.021 <0.012 0.077 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.009

0.10 0.018 0.012 0.008 0.054 0.020 0.008 0.058 0.018 0.008 0.053 0.104

0.447 0.304 0.232 0.064 0.656 0.163 0.07 0.42 0.122 0.067 0.302 Mandarin Misterbianc

o, Italy, 2005 Fruit

Fruit Fruit Fruit Pulp Peel Fruit Pulp Peel Fruit Pulp Peel 0*

0 7 14 14 14 21 21 21 28 28 28 0.02

0.19 0.06 0.04 <0.01 0.06 0.04 <0.01 0.10 0.03 <0.01 0.06 0.041

0.072 0.075 0.066 0.016 0.20 0.069 0.022 0.23 0.068 0.023 0.16 0.012

0.021 0.036 0.033 <0.012 0.11 0.034 <0.012 0.14 0.036 <0.012 0.096 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.008

0.011 0.008 0.014 <0.008 0.043 0.018 0.008 0.064 0.022 0.008 0.065 0.093

0.306 0.191 0.165 0.058 0.425 0.173 0.064 0.546 0.168 0.065 0.393



### MRL-calculation based on data obtained from the Sou thern Region: Both of the prescribed methods I and II have been u sed to calculate a proposed MRL for spirotetramat i n citrus fruits (based on data obtained from trials o f Southern Europe).

Individual data points for oranges are: 0.064 mg/kg, 0.064 mg/kg, 0.064 mg/kg, 0.069 mg/kg, 0.077 mg/kg, 0.114 mg/kg, 0.122 mg/kg and 0.233 mg/kg, Mean residue: 0.101 mg/kg; standard deviation: 0.05 8 mg/kg STMR: 0.07 mg/kg Highest residue: 0.233 mg/kg Method I: R max 

### = 0.287 mg/kg Method II: R ber 

### = 0.240 mg/kg Based on the data available for oranges, a MRL of 0 .3 mg/kg can be proposed.

Individual data points for mandarins are: 0.14 mg/kg, 0.146 mg/kg, 0.173 mg/kg, 0.185 mg/kg, 0.209 mg/kg, 0.232 mg/kg, 0.233 mg/kg, 0.273 mg/kg, 0.331 mg/kg Mean residue: 0.214 mg/kg; standard deviation: 0.06 2 mg/kg STMR: 0.209 mg/kg Highest residue: 0.331 mg/kg Method I: R max 

### = 0.401 mg/kg Method II: R ber 

### = 0.506 mg/kg Based on the data available for mandarins, a MRL of 0.5 mg/kg can be proposed..

### - 45 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

In the following calculation all available data for citrus fruits (combining oranges and mandarins)were considered: Mean residue: 0.153 mg/kg; standard deviation: 0.08 1 mg/kg STMR: 0.140 mg/kg Highest residue: 0.331 mg/kg Method I: R max 

### = 0.354 mg/kg Method II: R ber 

### = 0.441 mg/kg Based on the available data a MRL of 0.5 mg/kg for citrus fruits (whole group) can be proposed. Conclusion: In 17 residue trials on oranges and mandarins were carried out in Southern Europe. The residues in cit rus fruits (oranges and mandarins) 14 days after last t reatment (according to the intended uses) ranged be tween <0.054 mg/kg to 0.331 mg/kg. The different residue trials for citrus fruits were performed as residue decline studies with sampling intervals directly before the last application, 0, 7, 14, 21 and 28 days after t he last treatment. The critical trials with highest residue s levels were represented by the trials on mandarin s. According to the SANCO guidance document 7525/VI/95 -rev.7, 12/6/2001 it is possible to extrapolate fro m oranges and mandarins (8 trials each) to the whole group. Therefore the data are sufficient to propose an EU-MRL of 0.5 mg/kg for citrus fruits

. Comments (RMS): No comments.

B.7.6.2 Lettuce

Spirotetramat is applied for control of aphids in l ettuce. To demonstrate the residue situation on let tuce in Europe four studies in greenhouse (20 residue trial s), one field study in Northern Europe (4 trials) a nd one field study in Southern Europe (4 trials) were subm itted. Most of the residue trials were performed us ing 3 applications compared to 2 applications in the inte nded GAP. Details of the trial information are summ arized in Annex Ib. The intended European GAP is summarize d in Table B.7.6.2-1: Table B.7.6.2-1: GAP for residue situation in lettu ce North or South of EU Indoor or

outdoor Number of

applications Mode of

application Growth stage at

last application Application rate expressed

under the relevant unit PHI (d) EU-N F 2 Spray BBCH 48 0.072 g a.s./ha 7 EU-S F 2 Spray BBCH 48 0.072 g a.s./ha 7 EU-N/S G 2 Spray BBCH 48 0.072 g a.s./ha 7



### Reference: Determination of Residues of BYI08330 in/on Lettuce after Spraying of BYI08330 (150 OD) in the Greenhouse in Greece, Fran ce, Netherlands, Portugal Germany and Spain Author(s), year: Schöning R. ; 2006 Report/Doc. number: RA-2170/05, including trials no . R 2005 1023/3, R 2005 1024/1, R 2005 1026/8, R 2005 1027/6, R 2005 1028/4, R 2005 1029/2, R 2005 1 030/6, R 2005 1031/4 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: yes Deviations: no Validity: yes

### - 46 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Reference: Determination of Residues of BYI08330 in/on Lettuce after Spraying of BYI08330 (100 OD) in the Greenhouse in Germany, Sou thern France, Italy and Spain Author(s), year: Schöning R.; Wolters A.; 2005 Report/Doc. number: RA-2054/04, including trials no . R 2004 0393/3, R 2004 0394/1, R 2004 0396/8, R 20040397/6, R 2004 0398/4, R 2004 0399/2, R 2004 04 01/8, R 2004 0402/6 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: yes Deviations: no Validity: yes

Reference: Determination of Residues of BYI08330 in/on Lettuce after Spraying of BYI08330 (240 SC) in the Greenhouse in Germany, Ita ly and Spain Author(s), year: Schöning R.; Behn U.; 2005 Report/Doc. number: RA-2113/04, including trials no . R 2004 0685/1, R 2004 0687/8, R 2004 0688/6, R 2004 0689/4 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: yes Deviations: no Validity: yes

Reference: Determination of Residues of BYI08330 in/on Lettuce after Spraying of BYI08330 (100 OD) in the Field in the Netherlands a nd Germany Author(s), year: Schöning R.; Wolters A.; 2005 Report/Doc. number: RA-2052/04, including trials no . R 2004 0385/2, R 2004 0386/0, R 2004 0387/9, R 2004 0388/7 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: yes Deviations: no Validity: yes

Reference: Determination of Residues of BYI08330 in/on Lettuce after Spraying of BYI08330 (100 OD) in the Field in Southern France, Spain, Portugal and Italy Author(s), year: Schöning R.; Behn U.; 2005 Report/Doc. number: RA-2053/04, including trials no . R 2004 0389/5, R 2004 0390/9, R 2004 0391/7, R 2004 0392/5 M-260382-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: yes Deviations: no Validity: yes

Experimental design: The magnitude of residues of spirotetramat and its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-mono-hydroxy and BYI 08330-enol-Glc in/on let tuce harvested following the treatment with BYI 083 30

### - 47 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

formulations (100 OD, 150 OD and 240 SC) in greenho use (Greece, France, the Netherlander, Germany, Portugal and Spain) and under field conditions (N-E U: the Netherlands and Germany; S-EU: France, Spain

, Portugal and Italy) was determined. Overall 28 residue trials with BYI08330 in lettuce were conducted in 2004 and 2005. An overview on the supervised residue trials conducted with different formulations of BYI08330 is given in Table B.7.6.2- 2 Table B.7.6.2-2: Overview on European residue trial s with BYI08330 in lettuce

Location Formulation No. of trials Year Use rate

(g as/ha) Water volume No of appl. Spray interval

(days)

Greenhouse OD 100 8 2004 72 500-1000 3 7 Greenhouse OD 150 8 2005 72 500-1000 2 14 Greenhouse SC 240 + 0.2%

RME EW500 4 2004 72 500-1000 3 7

Field N-EU OD 100 4 2004 72 500-1000 3 7 Field S-EU OD 100 4 2004 72 500-1000 3 7



### In 2004, residue trials in lettuce were conducted i n the greenhouse (12 trials) and in the field in no rthern (4 trials) and in southern Europe (4 trials). These tr ials were not applied according to the intended Eur opean GAP. The different formulations were applied 3 time s with a spray interval of 7 days. The last applica tion was carried out at growth stage BBCH 32 – 49. The lettu ce samples were taken before the last treatment, 0, 1, 3 and 6-7 and 13-14 days after the last application. The greenhouse trials performed in 2005 were conduc ted with OD 150 formulation according the intended European GAP. The last applications were carried ou t at growth stage between BBCH 41 and BBCH 48. Samples were taken before the last application, 0, 1, 3, 7 and 14 days after the last application Different lettuce varieties were included in the re sidue trials. One half of the trials were conducted with head lettuce and the other half with loose-leaf varietie s. Analytical method used in all studies: Residues of spirotetramat and its metabolites BYI 0 8330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and BYI 08330-enol-Glc were determined by H PLC-ESI-MS/MS according to method 00857. The limit of quantification (LOQ, defined as the lowest validated fortificatio n level) was 0.01 mg/kg for spirotetramat, 0.012 mg/kg for its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and 0.008 mg/kg for BYI 08330-enol-Glc in/o n lettuce, calculated as spirotetramat equivalent. The mean procedural recoveries at the fortification levels of 0.01 to 10.0 mg/kg for spirotetramat and its four metabolites ranged between 84 and 96 %; these resul ts indicate that the methods used were suitable for this analysis. Findings: Most of the residue trials on lettuce were carried out with 3 applications per seasons. Number of appl ications and spray interval (6-8 days) in these submitted tr ials are not in accordance with the intended use fo r lettuce. 8 of the greenhouse trials in Europe are performed according to the intended GAP. As Test substance BY I 08330 100 OD was used in these trials. To evaluate the influence of different formulations of BYI 08330 (OD and SC) on the residue behaviour results was investigated by 8 greenhouse trials con ducted with the OD 100 formulation and 4 greenhouse trials conducted with the SC 240 formulation. In al l these trials 3 spray applications of BYI08330 for mulations were performed. There is no significant difference between these two formulation types (the results ar e listed in the table below). For the magnitude of spirotetramat residues under f ield conditions 4 trials from Northern Europe and f our trials from the Southern area were submitted. Altho ugh all trials were carried out using 3 spray appli cations and shorter spray intervals of 6-8 days in stead of 14 days, the residues resulting from these trials were generally lower as those found in the greenhouse tr ials according to the intended use. Therefore the greenhouse trials are considered as worst case situ ation concerning the residue behaviour. For MRL calculation the 8 residue trials were used, which w ere conducted with the OD150 formulation in the

### - 48 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

greenhouse according to the critical European use p attern. Total residues of spirotetramat in lettuce of between 0.163 and 2.33 mg/kg (STMR 1.23 mg/kg) were determined. The total residue of spirotetramat consists mainly of active substance and the enol metabolite. BYI083 30- ketohydroxy and –enol-glucoside are minor metabolit es. BYI08330-monohydroxy was not found. A detailed summary of the residue results is given in Appendix Ib.

Table B.7.6.2-3: Overview of European residue data for spirotetramat and its metabolites in lettuce used 2-3 times with application rates of 0.076 kg a .s./ha (residues are calculated as spirotetramat equivalent):

crop / No of appl./ fomulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330- keto hydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330

Greenhouse trials

Lettuce / 2 appl. 150 OD Kato Souli,

Greece, 2005 head

head head head head head 0*

0 1 3 7 14 0.10

1.5 1.6 1.4 0.70 0.58 0.12

0.31 0.37 0.40 0.26 0.28 0.026

0.039 0.057 0.063 0.053 0.053 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.027

0.025 0.033 0.034 0.032 0.046 0.285

1.886 2.072 1.909 1.057 0.971 Lettuce / 2 appl. 150 OD Quyilly,

France, 2005 head

head head head head head 0*

0 1 3 7 14 0.11

2.0 2.1 1.6 0.19 0.09 0.038

0.57 0.16 0.18 0.078 0.023 0.063

0.11 0.15 0.17 0.084 0.052 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.015

0.022 0.017 0.018 0.023 0.013 0.238

2.714 2.439 1.98 0.387 0.19 Lettuce / 2 appl. 150 OD RH Heiloo,

Netherlands, 2005 head

head head head head head 0*

0 1 3 7 14 0.45

1.6 1.5 1.4 1.3 0.87 0.18

0.34 0.30 0.29 0.35 0.26 0.063

0.067 0.085 0.082 0.086 0.066 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.713

2.027 1.905 1.792 1.756 1.216 Lettuce / 2 appl. 150 OD Torres

Vedras, Portugal, 2005 head

head head head head head 0*

0 1 3 7 14 <0.01

1.4 1.6 1.4 0.17 0.02 <0.012

1.0 0.38 0.33 0.12 0.043 <0.012

0.067 0.11 0.099 0.034 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

0.015 0.020 0.045 0.038 0.024 0.054

2.494 2.122 1.886 0.374 0.111 Lettuce / 2 appl. 150 OD St. Jory,

France, 2005 head

head 0

7 1.8

1.5 0.22

0.23 0.047

0.081 <0.012

<0.012 0.008

0.012 2.087

1.835

Lettuce / 2 appl. 150 OD Montfavet,

France, 2005 head

head 0

7 1.5

0.85 0.66

0.41 0.11

0.12 <0.012

<0.012 0.015

0.014 2.297

1.406

Lettuce / 2 appl. 150 OD Langenfeld,

Germany, 2005 head

head 0

7 1.3

0.05 0.30

0.056 0.014

0.031 <0.012

<0.012 0.008

0.014 1.634

0.163

Lettuce / 2 appl. 150 OD Bigues i

Riells, Spain, 2005 head

head 0

7 1.8

1.6 0.57

0.58 0.12

0.12 <0.012

<0.012 0.008

0.015 2.51

2.327

Lettuce / 3 appl. 100 OD Langenfeld,

Germany, 2004 head

head head head head head 0*

0 1 3 7 13 0.04

0.35 0.38 0.28 0.02 0.01 0.096

0.35 0.27 0.25 0.091 0.053 0.031

0.076 0.043 0.061 0.039 0.013 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.030

0.037 0.037 0.052 0.060 0.081 0.197

0.813 0.73 0.643 0.21 0.157

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / No of appl./ fomulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330- keto hydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330

Lettuce / 3 appl. 100 OD Jory,

Southern France, 2004 head

head head head head head 0*

0 1 3 7 14 0.07

0.49 0.63 0.06 0.02 0.01 0.12

0.69 0.32 0.18 0.080 0.031 0.041

0.16 0.090 0.047 0.025 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.022

0.042 0.027 0.038 0.059 0.067 0.253

1.382 1.067 0.325 0.184 0.12 Lettuce / 3 appl. 100 OD Leichlingen,

Germany, 2004 head

head head head 0

1 3 6 2.2

1.7 1.5 1.9 0.66

0.50 0.54 0.59 0.079

0.059 0.070 0.079 <0.012

<0.012 <0.012 <0.012 0.014

0.012 0.017 0.032 2.953

2.271 2.127 2.601 Lettuce / 3 appl. 100 OD Palidoro

Fiumicino, Italy, 2004 head

head head head 0

1 3 7 1.9

1.7 1.3 1.2 0.35

0.37 0.28 0.21 0.070

0.072 0.046 0.032 <0.012

<0.012 <0.012 <0.012 0.037

0.042 0.043 0.048 2.357

2.184 1.669 1.49 Lettuce / 3 appl. 100 OD Monopoli,

Italy, 2004 head

head head head head head 0*

0 1 3 6 14 1.7

5.9 5.1 3.7 2.6 0.60 0.49

0.73 0.68 0.76 0.53 0.24 0.13

0.14 0.14 0.17 0.15 0.079 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.051

0.056 0.052 0.13 0.15 0.093 2.371

6.826 5.972 4.76 3.43 1.012 Lettuce / 3 appl. 100 OD Bigues,

Spain, 2004 head

head head head head head 0*

0 1 3 7 14 0.54

1.4 1.2 0.73 0.52 0.39 0.52

0.75 0.71 0.60 0.51 0.22 0.18

0.24 0.22 0.22 0.17 0.081 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.057

0.058 0.071 0.067 0.084 0.074 1.297

2.448 2.201 1.617 1.284 0.765 Lettuce / 3 appl. 100 OD Monopoli,

Italy, 2004 head

head head head 0

1 3 7 2.2

1.1 1.4 1.0 0.55

0.35 0.31 0.27 0.18

0.11 0.093 0.096 <0.012

<0.012 <0.012 <0.012 0.056

0.037 0.049 0.067 2.986

1.597 1.852 1.433 Lettuce / 3 appl. 100 OD Brenes,

Spain, 2004 head

head head head 0

1 3 7 2.8

1.9 2.6 1.7 0.25

0.20 0.31 0.20 0.041

0.035 0.052 0.038 <0.012

<0.012 <0.012 <0.012 <0.008

<0.008 <0.008 0.008 3.091

2.135 2.962 1.946 Lettuce / 3 appl. 240 SC Langenfeld,

Germany, 2004 head

head head head head head 0*

0 1 3 7 13 0.02

0.42 0.5 0.31 0.03 0.01 0.088

0.38 0.29 0.21 0.1 0.054 0.023

0.093 0.048 0.037 0.028 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.036

0.042 0.051 0.056 0.07 0.084 0.179

0.947 0.901 0.625 0.24 0.172 Lettuce / 3 appl. 240 SC Monopoli,

Italy, 2004 head

head head head head head 0*

0 1 3 7 14 1.2

4.2 3.2 1.7 0.99 0.21 0.36

0.66 0.49 0.62 0.41 0.23 0.12

0.15 0.12 0.14 0.11 0.069 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.042

0.043 0.042 0.11 0.12 0.11 1.734

5.065 3.864 2.582 1.642 0.631 Lettuce / 3 appl. 240 SC Brenes,

Spain, 2004 head

head head head head 0*

0 1 3 7 1.1

1.8 2.2 1.7 1.5 0.15

0.21 0.29 0.18 0.21 0.036

0.032 0.05 0.044 0.044 <0.012

<0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 1.306

2.062 2.56 1.944 1.774 Lettuce / 3 appl. 240 SC Leichlingen,

Germany, 2004 head

head head head head 0*

0 1 3 6 1.2

2.1 1.8 1.6 1.5 0.19

0.28 0.25 0.27 0.21 0.064

0.081 0.089 0.08 0.066 <0.012

<0.012 <0.012 <0.012 <0.012 0.01

0.012 0.01 0.13 0.019 1.476

2.485 2.161 2.092 1.807

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / No of appl./ fomulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330- keto hydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 Field trials – Northern Europe

Lettuce / 3 appl. 150 OD ZwaagdijkOost, Netherlands, 2004 head

head head head head head 0*

0 1 3 7 14 0.03

0.53 0.46 0.37 0.17 0.03 0.085

0.15 0.18 0.2 0.1 0.026 0.05

0.05 0.057 0.064 0.082 0.019 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.033

0.031 0.04 0.057 0.077 0.063 0.21

0.773 0.749 0.703 0.441 0.15 Lettuce / 3 appl. 150 OD Langenfeld,

Germany, 2004 head

head head head 0

1 3 6 0.37

0.39 0.05 0.01 0.3

0.24 0.12 0.055 0.09

0.074 0.049 0.021 <0.012

<0.012 <0.012 <0.012 0.014

0.015 0.024 0.019 0.786

0.731 0.255 0.117 Lettuce / 3 appl. 150 OD BornheimSechten, Germany, 2004 head

head head head head head 0*

0 1 3 7 14 0.24

1.2 1.2 0.24 0.09 0.01 0.14

0.64 0.46 0.3 0.13 0.027 0.15

0.19 0.18 0.14 0.065 0.018 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.025

0.028 0.034 0.038 0.044 0.033 0.567

2.07 1.886 0.73 0.341 0.1 Lettuce / 3 appl. 150 OD Langenfeld,

Germany, 2004 head

head head head 0

1 3 6 0.58

0.13 0.01 0.01 0.45

0.26 0.11 0.068 0.062

0.057 0.059 0.028 <0.012

<0.012 <0.012 <0.012 0.029

0.028 0.039 0.033 1.133

0.487 0.23 0.151 Field trials – Southern Europe

Lettuce / 3 appl. 150 OD Lucenay,

France, 2004 head

head head head head head 0*

0 1 3 6 14 0.01

0.01 0.04 0.02 0.01 <0.01 0.046

0.054 0.13 0.076 0.043 0.013 0.022

0.024 0.034 0.028 0.017 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.011

0.012 0.02 0.024 0.024 0.022 0.101

0.112 0.236 0.16 0.106 0.069 Lettuce / 3 appl. 150 OD Vilanova del

Vallés, Spain, 2004 head

head head head 0

1 3 7 0.74

0.3 0.2 0.04 0.28

0.31 0.13 0.041 0.067

0.086 0.073 0.02 <0.012

<0.012 <0.012 <0.012 0.045

0.046 0.053 0.042 1.144

0.754 0.468 0.155 Lettuce / 3 appl. 150 OD Azueira,

Portugal, 2004 head

head head head head head 0*

0 1 3 7 14 0.03

1.3 0.4 0.33 0.05 0.02 0.071

0.52 0.32 0.19 0.078 0.029 0.025

0.056 0.083 0.085 0.028 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.018

0.02 0.021 0.021 0.02 0.014 0.156

1.908 0.836 0.638 0.188 0.087 Lettuce / 3 appl. 150 OD Bologna,

Italy, 2004 head

head head head 0

1 3 7 0.85

0.48 0.26 0.04 0.16

0.21 0.2 0.12 0.039

0.056 0.087 0.035 <0.012

<0.012 <0.012 <0.012 0.037

0.031 0.05 0.058 1.098

0.789 0.609 0.265



### For the calculation of the MRL proposal, both of th e prescribed methods I and II have been used for spirotetramat in lettuce (based on data obtained fr om trials from Northern and Southern Europe and glasshouse):

MRL-calculation based on data obtained from the Nor thern Region: Individual data points for lettuce are: 0.117 mg/kg, 0.151 mg/kg, 0.341 mg/kg and 0.441 mg/ kg Mean residue: 0.263 mg/kg; standard deviation: 0.15 5 mg/kg STMR: 0.25 mg/kg Highest residue: 0.441 mg/kg Method I: R max 

### = 1.057 mg/kg

### - 51 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Method II: R ber 

### = 0.832 mg/kg Based on the data available for lettuce in Northern Europe, a MRL of 1 mg/kg can be proposed.

MRL-calculation based on data obtained from the Sou thern Region: Individual data points for lettuce are: 0.106 mg/kg, 0.155 mg/kg, 0.188 mg/kg and 0.265 mg/ kg Mean residue: 0.179 mg/kg; standard deviation: 0.06 7 mg/kg STMR: 0.17 mg/kg Highest residue: 0.265 mg/kg Method I: R max 

### = 0.522 mg/kg Method II: R ber 

### = 0.492 mg/kg Based on the data available for lettuce in Southern Europe, a MRL of 0.5 mg/kg can be proposed.

MRL-calculation based on data obtained from the gre enhouse trials: Individual data points for lettuce are: 0.163 mg/kg, 0.374 mg/kg, 0.387 mg/kg, 1.057 mg/kg, 1.406 mg/kg, 1.756 mg/kg, 1.835 mg/kg and 2.327 mg/kg, Mean residue: 0.163 mg/kg; standard deviation: 0.79 8 mg/kg STMR: 1.23 mg/kg Highest residue: 2.33 mg/kg Method I: R max 

### = 3.706 mg/kg Method II: R ber 

### = 3.631 mg/kg Based on the data available for lettuce, a MRL of 5 mg/kg can be proposed.

Conclusion: All field trials and most of the greenhouse trials on lettuce were carried out with 3 applications per seasons. The number of applications and spray interval in th ese submitted trials are not in accordance with the intended GAP. Although the overdosed application in the field trials, the occurring residues were belo w the residues found in greenhouse trials according the i ntended GAP. Therefore the 8 the Europe greenhouse trials, performed according to the intended use and were taken for MRL calculation. Based on these tri als a MRL of 5 mg/kg can be proposed. Comments (RMS): No comments.

B.7.6.3 Pome fruit

Spirotetramat is applied for control of aphids, sca les, and mites in pome fruit. The critical European GAP for the use of BYI08330 in pome fruit in northern (N-EU ) and southern Europe (S-EU) is summarized in Table B.7.6.3-1 Table B.7.6.3-1: GAP for residue situation in pome fruit

North or South of EU Indoor or

outdoor Number of

applications Mode of

application Growth stage at

last application Application rate expressed

under the relevant unit PHI (d) EU-N F 2 Spray BBCH 81 0.072 kg a.s./ha and m canopy height, max. 0.216 kg a.s./ha 21

EU-S F 2 Spray BBCH 81 0.072 kg a.s./ha and m canopy height, max. 0.216 kg a.s./ha 21

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Reference: Determination of residues of BYI08330 in/on apple a nd pear after spraying and low-volume spraying of BYI08330 (100 OD) in the field in Germany, United Kingdom and Northern France Author(s), year: KIIA 6.3.1.3/01, Schöning R.; Helf rich P.; 2005 ; amended 12.01.2006 Report/Doc. number: RA-2135/04, including trials no . R 2004 0795/5, R 2004 0796/3, R 2004 0797/1, R 2004 0799/8 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: yes Deviations: no Validity: yes

Reference: Determination of residues of BYI08330 in/on apple a nd pear after spraying of BYI08330 (150 OD) in the field in United Kingdom an d Germany Author(s), year: Schöning R.; Eberhardt R ; 2006 Report/Doc. number: RA-2012/05, including trials no . R 2005 0083/1, R 2005 0085/8, R 2005 0086/6, R 2005 0087/4, R 2005 1018/7 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: no Validity: yes

Reference: Determination of residues of BYI08330 in/on apple a nd pear after spraying and low-volume spraying of BYI08330 (240 SC) in the field in Germany, United Kingdom and Northern France Author(s), year: Schöning R.; Helfrich P.; 2006 Report/Doc. number: RA-2138/04, including trials no . R 2004 0809/9, R 2004 0810/2, R 2004 0811/0, R 2004 0812/9 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: yes Deviations: no Validity: yes

Reference: Determination of residues of BYI08330 in/on apple a nd pear after spraying and low-volume spraying of BYI08330 (100 OD) in the field in Italy, Spain and southern France Author(s), year: Schöning R.; Helfrich P.; 2006 Report/Doc. number: RA-2137/04, including trials no . R 2004 0805/6, R 2004 0806/4, R 2004 0807/2, R 2004 0808/0 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: yes Deviations: no Validity: yes

### - 53 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Reference: Determination of residues of BYI08330 in/on apple a nd pear after spraying of BYI08330 (150 OD) in the field in United Kingdom an d Germany Author(s), year: Schöning R.; Eberhardt R ; 2006 Report/Doc. number: RA-2015/05, including trials no . R 2005 0088/2, R 2005 0089/0, R 2005 0090/4, R 2005 0091/2 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: no Validity: yes

Reference: Determination of residues of BYI08330 in/on apple a nd pear after spraying and low-volume spraying of BYI08330 (240 SC) in the field in Italy, Spain and southern France Author(s), year: Schöning R.; Helfrich P.; 2006 Report/Doc. number: RA-2136/04, including trials no . R 2004 0800/5, R 2004 0801/3, R 2004 0802/1, R 2004 0804/8 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: yes Deviations: no Validity: yes

Experimental design For the Northern European region 13 residue decline trials (Germany, France and UK) were conducted. Ni ne of these trials were performed using oil based disp ersion concentrates containing 150 g/L and 100 g/L of spirotetramat. The remaining four trials were carri ed out with a suspension concentrate containing 240 g spirotetramat/L. In three of these trials the Addit ive RME 500 EW was added. For Southern Europe 12 residue trials were performe d in Italy, Spain and S-France. Four trials each we re performed with the three different formulations men tioned in the table below. In 3 of these 8 trials conducted with the SC 240 fo rmulation of spirotetramat the additive RME EW500 w as not added at the recommended concentration of 0.2 % : RME was not added to the spray liquid at all (R 2 004 0810/2), it was added to the spray liquid at the se cond application (R2004 0811/0), only, or was added at both applications at a reduced rate of 0.14 % (R 20 04 0804/8). The product was used twice with an application rate of 0.072 kg a.s./ha and meter height of leaf surfa ce (2 – 3 m), resulting application rates between 0.144 and 0.2160 kg a.s./ha. All trials were performed accor ding to the critical European GAP. Due to different agricultural practices in European countries different rates of water are used for sp ray applications in pome fruit. In most cases a water r ate of 500 L/ha x m canopy height (CH) was used. To cover the low volume application technique, in 4 tr ials a water volume of 250-300 L/ha x m CH was appl ied, while keeping the rate for the active substance at 72 g/ ha x m CH. An overview on the supervised residue trials is giv en in Table B.7.6.3-2.

Table B.7.6.3-2: Overview on supervised residue tr ials with BYI08330 in pome fruit

Study no. Region Formulation No. of

trials Year Use rate (g as/ha x m CH) Water

volume (L/ha x m CH) (a) No of

appl. Spray

interval (days) PHI

days

RA-2135/04 N-EU OD 100 4 2004 72 300/500 2 14 21 RA-2138/04 N-EU OD150 4 2004 72 300/500 2 14 21 RA-2012/05 N-EU OD 150 5 2005 72 500 2 14 21

### - 54 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Study no. Region Formulation No. of

trials Year Use rate (g as/ha x m CH) Water

volume (L/ha x m CH) (a) No of

appl. Spray

interval (days) PHI

days

RA-2137/04 S-EU SC 240 4 2004 72 250/500 2 14 21 RA-2136/04 S-EU SC 240 4 2004 72 250/500 2 14 21 RA-2015/05 S-EU OD150 4 2005 72 500 2 14 21



### The second application was carried out at BBCH grow th stage 77-85. Apple and pear samples were taken before the last a pplication, 0, 7, 14, 21 and 28 days after the last application. In one study, in addition leaf samples were taken at 0, 2-3, 6-7 and 14 days after treatm ent. Analytical method used in all studies: Residues of spirotetramat and its metabolites BYI 0 8330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and BYI 08330-enol-Glc were determined by H PLC-ESI-MS/MS according to method 00857. Residues of spirotetramat and its metabolites BYI 0 8330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and BYI 08330-enol-Glc were extracted from the sample material using with acidic acetonitrile/ water mixture (4/1, v/v). After filtration of the e xtract, the residues were quantified by reversed ph ase HPLC with Electro spray and MS/MS detection without any further clean-up step. The quantification was perfo rmed using a stable-labelled internal standard for each reference item. The limit of quantification (LOQ, defined as the lowest validated fortificatio n level) was 0.01 mg/kg for spirotetramat, 0.012 mg/kg for its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and 0.008 mg/kg for BYI 08330-enol-Glc in/o n apples and pears, calculated as spirotetramat equivalent. The mean procedural recoveries at the fortification levels of 0.01 to 10.0 mg/kg for spirotetramat and its four metabolites ranged between 86 and 106 %; these resu lts indicate that the methods used were suitable fo r this analysis. Findings: A detailed summary of the residue trial for apples and pears is given in Annex Ic. The total residue of spirotetramat in apple and pea r fruit from residue trials in Northern Europe afte r two applications ranged between 0.064 mg/kg and 0.254 m g/kg. Residues in pome fruit from southern European residue trials were very similar ranging between <0 .054 mg/kg (LOQ) and 0,249 mg/kg. Moreover, an influence of different formulations (O D100, OD150, SC240 with and without RME) or of the amount of water used for the spray application on t he height of residues could not be observes. An overview of the European residue data for spirot etramat and its metabolites is given in the table b elow.

Table B.7.6.3-3: Overview of European residue data for spirotetramat and its metabolites in pome fruit used 2 times with application rates of 0.076 kg a.s./ha and meter canopy height (residues are calculated as spirotetramat equivalent):

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330- keto hydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 Northern Europe Apple / 100 OD Burscheid,

Germany, 2004 fruit

fruit fruit fruit 0

13 21 27 0.10

0.02 0.01 0.02 <0.012

0.016 0.012 0.012 0.012

0.014 0.012 0.017 <0.012

<0.012 <0.012 0.012 < 0.008

< 0.008 < 0.008 0.008 0.144

0.070 0.054 0.069 Apple / 100 OD Royston,

United Kingdom, 2004 fruit

fruit fruit fruit fruit fruit 0

0 7 13 21 28 0.07

0.21 0.12 0.07 0.04 0.02 0.014

0.017 0.025 0.026 0.034 0.033 0.012

0.012 0.018 0.013 0.021 0.025 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.116

0.259 0.183 0.129 0.115 0.098

### - 55 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330- keto hydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 apple / 150 OD Essex, UK,

2005 fruit

leaf leaf leaf fruit leaf fruit fruit 0

0 3 6 14 14 21 29 0.11

9.5 6.2 5.5 0.05 3.2 0.03 0.01 0.023

0.77 0.35 0.6 0.031 0.17 0.034 0.021 0.012

0.59 1.1 1.1 0.014 1.3 0.015 0.019 <0.012

0.012 0.012 0.012 <0.012 0.012 <0.012 <0.012 <0.008

0.008 0.008 0.01 <0.008 0.011 <0.008 <0.008 0.165

10.88 7.67 7.222 0.115 4.693 0.099 0.07 apple / 150 OD Bernau,

Germany, 2005 fruit

fruit leaf leaf fruit leaf fruit leaf fruit fruit 0*

0 0 2 7 7 14 14 21 28 0.02

0.12 13 9.6 0.1 7.2 0.03 2.2 0.03 0.02 0.016

0.017 0.79 0.75 0.022 0.28 0.019 0.093 0.021 0.012 0.012

0.012 0.76 1.2 0.015 1.1 0.018 0.64 0.023 0.017 <0.012

<0.012 0.019 0.024 0.012 0.039 0.012 0.043 0.012 0.012 <0.008

<0.008 0.008 0.01 <0.008 0.017 <0.008 0.018 0.008 <0.008 0.068

0.169 14.577 11.584 0.157 8.636 0.087 2.994 0.094 0.069 apple / 150 OD WurzenRoitzsch, Germany, 2005 fruit

fruit fruit fruit 0

15 22 29 0.14

0.08 0.07 0.06 0.022

0.049 0.052 0.037 0.012

0.012 0.013 0.012 <0.012

0.012 0.012 0.012 <0.008

<0.008 0.008 0.008 0.194

0.161 0.155 0.129 apple / 240 SC Burscheid,

Germany, 2004 fruit

fruit fruit fruit 0

14 21 28 0.13

0.01 0.02 0.01 <0.012

0.012 0.012 0.012 <0.012

<0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.008

<0.008 0.008 <0.008 0.174

0.054 0.064 0.054 apple / 240 SC Royston,

UK, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 7 13 21 28 0.02

0.23 0.06 <0.01 0.02 0.01 <0.012

0.012 0.012 <0.012 0.012 0.012 <0.012

0.012 0.012 <0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.064

0.274 0.104 0.054 0.064 0.054 pear / 100 OD Burscheid,

Germany, 2004 fruit

fruit fruit fruit 0

13 21 27 0.15

0.02 0.02 0.01 0.012

<0.012 <0.012 <0.012 0.012

0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 0.194

0.064 0.064 <0.054 pear / 100 OD Ecquevilly,

France, 2004 fruit

fruit fruit fruit fruit fruit 0

0 6 13 21 27 0.03

0.14 0.06 0.06 0.05 0.03 <0.012

0.012 0.012 0.012 0.012 <0.012 <0.012

<0.012 0.012 0.012 0.012 0.012 0.012

0.012 0.012 0.012 0.012 0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.074

0.184 0.104 0.104 0.094 0.074 pear / 150 OD Cambridge,

UK, 2005 fruit

leaf leaf leaf fruit leaf fruit fruit 0

0 3 7 14 14 21 28 0.38

24 19 5.4 0.08 3.5 0.05 0.04 0.024

1.5 0.56 0.24 0.012 0.13 0.012 0.012 0.012

0.37 0.97 0.45 0.022 0.37 0.016 0.012 0.012

0.037 0.072 0.084 0.012 0.083 0.012 0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 0.436

25.915 20.61 6.182 0.134 4.091 0.098 0.084

### - 56 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330- keto hydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 pear / 150 OD Geisenheim

Germany, 2005 fruit

fruit leaf leaf fruit leaf fruit leaf fruit fruit 0*

0 0 3 7 7 14 14 21 28 0.04

0.25 24 22 0.22 19 0.14 13 0.1 0.06 0.012

0.023 1.5 0.43 0.013 0.56 0.012 0.44 0.012 0.012 0.012

0.012 0.5 0.78 0.013 0.53 0.017 0.77 0.016 0.014 0.013

0.014 0.23 0.21 0.02 0.22 0.021 0.25 0.02 0.021 <0.008

<0.008 0.008 0.009 0.008 0.008 0.008 0.008 0.008 <0.008 0.085

0.307 26.238 23.429 0.274 20.318 0.198 14.468 0.156 0.115 pear / 240 SC Burscheid,

Germany, 2004 fruit

fruit fruit fruit 0

13 21 27 0.18

0.15 0.14 0.14 0.039

0.034 0.033 0.031 0.035

0.033 0.029 0.027 0.053

0.046 0.044 0.043 0.008

0.008 0.008 0.008 0.315

0.271 0.254 0.249 pear / 240 SC Ecquevilly,

N-France, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 6 13 21 27 0.03

0.19 0.11 0.06 0.07 0.05 <0.012

0.012 0.012 0.012 0.012 <0.012 <0.012

0.012 0.012 0.012 0.012 0.012 <0.012

<0.012 0.012 0.012 0.012 0.012 <0.008

<0.008 <0.008 <0.008 <0.008 0.008 0.074

0.234 0.154 0.104 0.114 0.094 Southern Europe apple / 100 OD Mirobello,

Italy, 2004 fruit

fruit fruit fruit 0

14 21 28 0.30

0.06 0.04 0.05 0.019

0.015 0.014 0.013 0.012

0.012 0.012 0.012 <0.012

<0.012 <0.012 0.012 <0.008

<0.008 <0.008 <0.008 0.351

0.107 0.086 0.095 pear / 100 OD Merelli,

Italy, 2004 fruit

fruit fruit fruit 0

14 21 28 0.27

0.10 0.07 0.10 0.033

0.012 0.012 0.012 0.02

0.019 0.013 0.019 <0.012

<0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 0.343

0.151 0.115 0.151 apple / 100 OD Vilamacolu

m, Spain, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 10 14 20 27 0.09

0.23 0.20 0.12 0.10 0.05 0.013

0.016 0.023 0.022 0.015 0.012 0.019

0.02 0.034 0.034 0.041 0.032 0.017

0.016 0.027 0.025 0.028 0.021 <0.008

0.008 0.008 0.008 0.008 0.008 0.147

0.29 0.292 0.209 0.192 0.123

pear – 100 OD Les Chères,

S-France, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 7 14 21 28 0.12

0.38 0.18 0.15 0.14 0.14 0.030

0.063 0.038 0.033 0.033 0.032 0.026

0.039 0.034 0.031 0.027 0.027 0.032

0.13 0.053 0.045 0.041 0.041 0.008

0.008 0.008 0.008 0.008 0.008 0.216

0.62 0.313 0.267 0.249 0.248 apple / 150 OD SaintPardoux, SFrance, 2005 fruit

fruit fruit fruit fruit fruit 0*

0 7 14 21 28 0.03

0.11 0.08 0.04 0.04 0.03 0.012

0.012 0.012 0.013 0.022 0.02 <0.012

<0.012 0.012 0.012 0.014 0.023 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.074

0.154 0.124 0.085 0.096 0.093 apple / 150 OD Bologna,

Italy, 2005 fruit

fruit fruit fruit 0

14 21 28 0.11

0.06 0.08 0.02 0.012

0.012 0.012 0.012 0.012

0.012 0.015 0.012 0.012

0.012 0.014 0.012 <0.008

0.008 0.008 0.008 0.154

0.104 0.129 0.064

pear – 150 OD Grenade, SFrance, 2005 fruit

fruit fruit fruit fruit fruit 0*

0 7 14 21 28 0.04

0.14 0.05 0.05 0.02 0.02 0.012

0.022 0.012 0.012 0.012 <0.012 0.02

0.016 0.029 0.029 0.022 0.018 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.092

0.198 0.111 0.111 0.074 0.070

### - 57 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330- keto hydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330

pear – 150 OD Albaro Di

Ronco All’Adige, Italy, 2005 fruit

fruit fruit fruit 0

14 21 28 0.11

0.03 0.02 0.01 0.012

<0.012 <0.012 <0.012 0.012

0.014 0.014 <0.012 <0.012

<0.012 0.012 0.012 <0.008

<0.008 <0.008 <0.008 0.154

0.076 0.066 <0.054 apple / 240 SC + 0.2 % RME 500 EW Mirabello,

Italy, 2004 fruit

fruit fruit fruit 0

14 21 28 0.35

0.04 0.01 0.01 0.019

0.012 0.012 0.012 0.015

0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 0.404

0.084 <0.054 0.054 pear / 240 SC + 0.2 % RME 500 EW Dodici

Morelli, Italy, 2004 fruit

fruit fruit fruit 0

14 21 28 0.22

0.1 0.08 0.09 0.032

0.012 0.012 0.012 0.012

0.024 0.018 0.018 <0.012

<0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 0.284

0.156 0.13 0.14 apple / 240 SC + 0.2 % RME 500 EW Vilamacolu

m, Spain, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 10 14 20 27 0.14

0.33 0.25 0.11 0.09 0.05 0.012

0.012 0.012 0.013 0.012 0.012 0.012

0.012 0.017 0.019 0.022 0.014 0.012

0.012 0.012 0.012 0.012 0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.184

0.374 0.299 0.162 0.144 0.096

pear – 240 SC + 0.14 % RME 500 EW Les Chères,

S-France, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 7 14 21 28 <0.01

0.14 0.02 <0.01 0.01 <0.01 <0.012

0.012 <0.012 <0.012 <0.012 <0.012 <0.012

0.012 0.012 <0.012 0.012 <0.012 <0.012

0.012 0.012 <0.012 0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.054

0.184 0.064 0.054 <0.054 0.054



### The parent compound generally covered the main part of the total residue of spirotetramat. The enol an d the ketohydroxy metabolite were also present at minor a mounts. The monohydroxy metabolite was detected as minor metabolite in some trials. The enol-glucoside metabolite in pome fruit was only found in traces. According to the guidance document SANCO 7525/VI/95 /rev.7, table 3, it is possible to extrapolate from apples or pears (with a minimum of 4 apples trials) to the whole group of pome fruit. Therefore all re sults of apples and pears were taken for the calculation of the MRL proposal. Both of the prescribed methods I and II have been used for MRL calculation for spirotetrama t in pome fruit (based on data obtained from trials from Northern and Southern Europe):

MRL-calculation based on data obtained from the Nor thern Region: Individual data points for apple are: 0.064 mg/kg, 0.064 mg/kg, 0.069 mg/kg, 0.094 mg/kg, 0.099 mg/kg, 0.115 mg/kg, 0.155 mg/kg, Individual data points for pear are: 0.064 mg/kg, 0.094 mg/kg, 0.098 mg/kg, 0.114 mg/kg, 0.156 mg/kg, 0.254 mg/kg, Mean residue: 0.111 mg/kg; standard deviation: 0.05 3 mg/kg STMR: 0.098 mg/kg Highest residue: 0.254 mg/kg Method I: R max 

### = 0.252 mg/kg Method II: R ber 

### = 0.270 mg/kg Based on the data available for pome fruit in North ern Europe, a MRL of 0.3 mg/kg can be proposed.

MRL-calculation based on data obtained from the Sou thern Region: Individual data points for apple are: <0.054 mg/kg, 0.095 mg/kg, 0.096 mg/kg, 0.129 mg/kg , 0.144 mg/kg, 0.192 mg/kg, Individual data points for pear are: <0.054 mg/kg, 0.066 mg/kg, 0.074 mg/kg, 0.14 mg/kg, 0.151 mg/kg, 0.249 mg/kg

### - 58 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Mean residue: 0.120 mg/kg; standard deviation: 0.05 9 mg/kg STMR: 0.11 mg/kg Highest residue: 0.249 mg/kg Method I: R max 

### = 0.283 mg/kg Method II: R ber 

### = 0.299 mg/kg Based on the data available for pome fruit in south ern Europe, a MRL of 0.3 mg/kg can be proposed.

Conclusion: In 2004 and 2005, altogether 25 residue trials were conducted in pome fruit (apples and pears) in Nort hern and Southern Europe using three different formulati ons of spirotetramat, the OD 100, the OD 150 and th e SC 240 + 0.2 % RME EW 500. All trials were performed a ccording to the intended European GAP. The residues in pome fruit from northern and southe rn Europe were very similar and resulted in the sam e MRL of 0.3 mg/kg. The highest residue in N-EU reach ed 0.254 mg/kg whereas in S-EU 0.249 mg/kg were found. In general no influence of the different loc ations (S-EU/N-EU) on the residue behaviour could b e detected. Comments (RMS): No comments.

B.7.6.4 Stone fruit

B.7.6.4.1 Peach and apricot

Spirotetramat is applied for control of aphids, sca les, and mites in peaches and apricots. The critica l European GAP for the use in northern (N-EU) and sou thern Europe (S-EU) is summarized in Table B.7.6.4.1-1 Table B.7.6.4-1: GAP for residue situation in peach and apricot

North or South of EU Indoor or

outdoor Number of

applications Mode of

application Growth stage at

last application Application rate expressed

under the relevant unit PHI (d) EU-N F 2 Spray BBCH 81 0.072 kg a.s./ha and m canopy height, max. 0.216 kg a.s./ha 21

EU-S F 2 Spray BBCH 81 0.072 kg a.s./ha and m canopy height, max. 0.216 kg a.s./ha 21



### Reference: Determination of Residues of BYI08330 in/on Peach a nd Apricot after Spraying of BYI08330 (100 OD) in the Field in North ern France and Germany Author(s), year: Schöning R.; Wolters A.; 2005 Report/Doc. number: RA-2126/04, including trials no. R 2004 0785/8, R 2004 0786/6 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: yes Deviations: no Validity: yes

### - 59 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Reference: Determination of Residues of BYI08330 in/on Peach a nd Apricot after Spraying of BYI08330 (150 OD) in the Field in Germa ny and Northern France Author(s), year: Schöning R.; Eberhardt R.; 2006 Report/Doc. number: RA-2006/05, including trials no . R 2005 0059/9, R 2005 0060/2, R 2005 0061/0 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: yes Deviations: no Validity: yes

Reference: Determination of Residues of BYI08330 in/on Peach a nd Apricot after Spraying of BYI08330 (100 OD) in the Field in Spain and Italy Author(s), year: Schöning R.; Helfrich P.; 2006 Report/Doc. number: RA-2127/04, including trials no . R 2004 0787/4, R 2004 0788/2, R 2004 0789/0, R 2004 0790/4 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: yes Deviations: no Validity: yes

Reference: Determination of Residues of BYI08330 in/on Apricot and Peach after Spraying of BYI08330 (150 OD) in the Field in Portu gal, Spain, Greece, Southern France and Italy Author(s), year: Schöning R.; Eberhardt R.; 2006 Report/Doc. number: RA-2007/05, including trials no . R 2005 0062/9, R 2005 0063/7, R 2005 0064/5, R 2005 0065/3, R 2005 0066/1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: yes Deviations: no Validity: yes

Experimental design For the Northern Europe, 5 residue decline trials ( Germany and N-France) on apricot and peaches were conducted. Only two of these trials were carried ou t on peaches. Peaches and apricots are classified as minor crop i n northern Europe and as major crop in southern Eur ope, but according to guidance document SANCO 7525/VI/95 /rev.7, four trials are necessary to support a use for minor crops and extrapolation from peaches or apric ots to the group nectarines, apricots and peaches c an only be made with a minimum or 4 peaches trials. In Southern Europe 9 residue trials (4 on peaches a nd 5 on apricots) were performed in Italy, Spain, Portugal, Greece and S-France. All studies were carried out using oil based disper sion concentrates containing 150 g/L and 100 g/L of spirotetramat. The product was used twice with an application rate of 0.072 kg a.s./ha and meter height of leaf surfa ce (2 – 3 m), resulting application rates between 0.144 and 0.2160 kg a.s./ha. All trials were performed accor ding to the critical European GAP. Due to different agricultural practices in European countries different rates of water are used for sp ray applications. In most cases a water rate of 500 L/h a x m canopy height (CH) was used. To cover the low

### - 60 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

volume application technique, in one trial (Norther n Europe) a water volume of 300 L/ha and meter cano py height was applied, while keeping the rate for the active substance at 72 g/ ha x m canopy height. An overview on the supervised residue trials is giv en in Table B.7.6.4-2.

Table B.7.6.4-2: Overview on supervised residue tr ials with BYI08330 in peach and apricot

Study no. Region Formulation No. of

trials Year Use rate (g as/ha x m CH) Water

volume (L/ha x m CH) (a) No of

appl. Spray

interval (days) PHI

days

RA-2126/04 N-EU OD 100 2 2004 72 500 2 14 21 RA-2006/05 N-EU OD150 3 2005 72 300/500 2 14 21 RA-2127/04 S-EU OD 100 4 2004 72 500 2 14-16 21-22 RA-2007/05 S-EU OD150 5 2005 72 500 2 14 20-21



### The second application was carried out at BBCH grow th stages 75-81. Apricot and peach samples were taken before the las t application, 0, 7, 14, 21 and 28 days after the l ast application. Analytical method used in all studies: The residues of spirotetramat and its metabolites B YI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-mon ohydroxy and BYI 08330-enol-Glc in peach and apricot were determined by HPLC-ESI-MS/MS according to method 00857. The limit of quantification (LOQ, defined as the lowest validated fortificatio n level) was 0.01 mg/kg for spirotetramat, 0.012 mg/kg for its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and 0.008 mg/kg for BYI 08330-enol-Glc in/o n peaches and apricots, calculated as spirotetramat equivalent. The mean procedural recoveries at the fortification levels of 0.01 to 2.0 mg/kg f or spirotetramat and its four metabolites ranged between 83 and 102 % and RSD < 2 0%; these results indicate that the methods used were suitable for this analysis. Findings: A detailed summary of the residue trial for peaches and apricots is given in Annex Id. For Northern Europe, only two residue trials on pea ches and three trials on apricots were submitted to demonstrate the residue situation in peaches and ap ricots according the intended European GAP. Peaches and apricots are classified as minor crop i n northern Europe and as major crop in southern Eur ope, but according to guidance document SANCO 7525/VI/95 /rev.7, four trials are necessary to support a use for minor crops and extrapolation from peaches or apric ots to nectarines, apricots and peaches can only be made with a minimum or 4 peaches trials. Results from residue trials in Southern Europe cond ucted according to the intended European GAP showed total residues of 0.115 to 0.687 mg/kg (STMR 0.345 mg/kg) in peaches and apricots sampled at the PHI o f 21 days after 2 applications of BYI 08330 formulati ons. The enol metabolite is a major component of the tot al residue in peaches and apricots appearing at amo unts between 0.047 and 0.29 mg/kg. In peaches minor meta bolites were the parent compound, the monohydroxy and ketohydroxy metabolites; the enol-glucoside met abolite was detected in traces only. In apricots th e enolglucoside metabolite was detected at 0.11-0.43 mg/k g and could occur in similar amounts as the enol metabolite; the monohydroxy metabolite was detected in traces, only. An overview of the European residue data for spirot etramat and its metabolites is given in the table b elow.

### - 61 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.6.4-3: Overview of European residue data for spirotetramat and its metabolites in peaches and apricots used 2 times with application rates of 0.076 kg a.s./ha and meter canopy height (residues are calculated as spirotetramat equivalen t):

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 Northern Europe peach / OD 100 Pouligny

SaintPierre, NFrance, 2004 fruit

fruit fruit fruit 0

14 21 27 0.51

0.10 0.07 0.07 0.13

0.24 0.15 0.15 0.053

0.041 0.029 0.032 0.036

0.057 0.053 0.053 0.009

0.013 0.012 0.012 0.738

0.451 0.314 0.317

apricot / OD 100 Geisenheim

, Germany, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 7 14 21 28 0.07

0.26 0.17 0.12 0.14 0.09 0.074

0.094 0.14 0.12 0.095 0.077 0.019

0.016 0.018 0.013 0.014 0.013 0.012

0.012 0.012 0.012 0.012 0.012 0.15

0.11 0.18 0.21 0.25 0.28 0.325

0.492 0.520 0.475 0.511 0.472 apricot / OD 150 Höhnstedt,

Germany, 2005 fruit

fruit fruit 0

14 21 0.39

0.07 0.04 0.25

0.37 0.29 0.058

0.044 0.034 0.012

0.012 0.012 0.26

0.37 0.32 0.970

0.866 0.696 apricot / OD 150 Geisenheim

, Germany, 2005 fruit

fruit fruit fruit fruit 0*

0 7 14 21 0.10

0.29 0.15 0.08 0.07 0.085

0.092 0.19 0.21 0.13 0.012

0.012 0.014 0.016 0.018 0.012

0.012 0.012 0.012 0.012 0.082

0.086 0.17 0.24 0.29 0.291

0.492 0.536 0.558 0.520 peach / OD 150 Pouligny

SaintPierre, NFrance, 2005 fruit

fruit fruit fruit fruit fruit 0*

0 7 14 21 27 0.12

0.26 0.14 0.10 0.06 0.04 0.080

0.088 0.25 0.24 0.25 0.18 0.032

0.032 0.042 0.033 0.035 0.027 0.012

0.012 0.062 0.074 0.083 0.065 <0.008

<0.008 0.008 0.009 0.010 0.009 0.252

0.400 0.502 0.456 0.438 0.321 Southern Europe peach / OD 100 La Fortesa,

Spain, 2004 fruit

fruit fruit fruit 0

14 22 27 0.48

0.08 0.04 0.02 0.23

0.28 0.19 0.13 0.057

0.037 0.027 0.020 0.03

0.092 0.081 0.087 0.008

0.008 0.008 0.008 0.805

0.497 0.346 0.265 apricot / OD 100 Bologna,

Italy, 2004 fruit

fruit fruit fruit 0

14 21 28 0.42

0.08 0.07 0.04 0.27

0.23 0.14 0.086 0.041

0.03 0.023 0.020 0.012

0.014 0.016 0.015 0.22

0.37 0.43 0.40 0.963

0.724 0.679 0.561 peach / OD 100 Ravenna,

Italy, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 7 14 21 28 0.08

0.33 0.15 0.05 0.03 0.01 0.048

0.068 0.12 0.10 0.071 0.044 0.044

0.046 0.050 0.034 0.017 0.012 0.023

0.028 0.039 0.040 0.044 0.039 0.008

0.009 0.009 0.008 0.008 0.008 0.203

0.481 0.368 0.232 0.170 0.113 apricot / OD 100 Pobla del

Duc, Spain, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 7 14 21 28 0.01

0.16 0.07 0.04 0.02 0.02 0.048

0.074 0.093 0.099 0.13 0.091 0.012

0.022 0.023 0.015 0.014 0.012 <0.012

<0.012 <0.012 <0.012 0.012 0.012 0.036

0.050 0.073 0.077 0.11 0.12 0.118

0.318 0.271 0.243 0.286 0.255 apricot / OD 150 Mato,

Portugal, 2005 fruit

fruit fruit fruit 0

14 21 28 0.61

0.21 0.09 0.10 0.40

0.30 0.16 0.11 0.094

0.097 0.085 0.050 0.012

0.012 0.012 0.012 0.12

0.34 0.34 0.33 1.236

0.959 0.687 0.602

### - 62 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 peach / OD 150 La Fortesa,

Spain, 2005 fruit

fruit fruit fruit 0

13 20 28 0.35

0.19 0.09 0.06 0.062

0.15 0.093 0.071 0.034

0.048 0.016 0.012 0.020

0.097 0.10 0.11 0.008

0.008 0.008 0.008 0.474

0.493 0.307 0.261 apricot / OD 150 Souli

Korinthias, Greece, 2005 fruit

fruit fruit fruit 0

14 21 28 0.25

0.15 0.05 0.05 0.064

0.094 0.063 0.039 0.012

0.012 0.012 0.012 <0.012

<0.012 0.012 <0.012 0.046

0.10 0.099 0.10 0.384

0.368 0.236 0.213 peach / OD 150 Montfavet,

S-France, 2005 fruit

fruit fruit fruit fruit fruit 0*

0 7 14 21 28 0.04

0.22 0.09 0.05 0.03 0.02 0.037

0.061 0.11 0.071 0.047 0.054 0.022

0.022 0.023 0.014 0.012 0.012 0.012

0.012 0.019 0.022 0.018 0.019 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.119

0.323 0.25 0.165 0.115 0.113 apricot / OD 150 Bologna,

Italy, 2005 fruit

fruit fruit fruit fruit fruit 0*

0 7 14 21 27 0.04

0.12 0.05 0.03 0.02 0.02 0.058

0.079 0.14 0.10 0.061 0.040 0.012

0.014 0.015 0.012 0.012 0.013 <0.012

0.012 0.012 0.012 0.012 0.012 0.064

0.074 0.099 0.11 0.17 0.16 0.186

0.299 0.316 0.264 0.275 0.245



### According to the SANCO guidance document 7525/VI/95 /rev. 7, it is possible to extrapolate from peaches or apricots (with a minimum of 4 peaches trials) to ne ctarines, apricots and peaches. Therefore all resul ts of peaches and apricots were taken for the calculation of the MRL proposal for Southern Europe. For the Northern region no extrapolation is possible accord ing the above mentioned guidance paper. For a MRL proposal for the single commodities a minimum numbe r of four trials is requested, therefore a MRL-prop osal was calculated not calculated for Northern Europe, because of the lack of data. Both of the prescribed methods I and II have been u sed for MRL calculation for spirotetramat in peache s and apricots (based on data obtained from trials from S outhern Europe):

MRL-calculation based on data obtained from the Sou thern Region: Individual data points for peach are: 0.115 mg/kg, 0.17 mg/kg, 0.307 mg/kg, 0.346 mg/kg Individual data points for apricot are: 0.236 mg/kg, 0.275 mg/kg, 0.286 mg/kg, 0.679 mg/kg, 0.687 mg/kg

Mean residue: 0.345 mg/kg; standard deviation: 0.20 4 mg/kg STMR: 0.29 mg/kg Highest residue: 0.687 mg/kg Method I: R max 

### = 0.964 mg/kg Method II: R ber 

### = 1.025 mg/kg Based on the data available for peaches, nectarins and apricots in Southern Europe, a MRL of 1 mg/kg can be proposed.

Conclusion: In 2004 and 2005, altogether 14 residue trials were conducted on peach and apricot in Northern and Southern Europe using two different formulations of spirotetramat (OD 100 and OD 150). All trials were performed according to the intended European GAP.

### - 63 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

For Northern Europe 3 trials on apricot and only tw o trials on peaches were submitted. According to guidance document guidance document SANCO 7525/VI/9 5-rev.7, there are no sufficient data available to describe the residue situation in Northern Europe. The residues in peach and apricot from Southern Eur ope resulted in the MRL of 2 mg/kg. The highest residue in S-EU reached 0.254 mg/kg. Comments (RMS): No comments.

B.7.6.4.2 Plum

Spirotetramat is applied for the use in plums for t he control of aphids, scales, and mites. The critic al European GAP for the use in northern (N-EU) and sou thern Europe (S-EU) is summarized in Table B.7.6.4.2-1. Table B.7.6.4.2-1: GAP for residue situation in plu m North or South of EU Indoor or

outdoor Number of

applications Mode of

application Growth stage at

last application Application rate expressed

under the relevant unit PHI (d) EU-N F 2 Spray BBCH 81 0.072 kg a.s./ha and m canopy height, max. 0.216 kg a.s./ha 21

EU-S F 2 Spray BBCH 81 0.072 kg a.s./ha and m canopy height, max. 0.216 kg a.s./ha 21



### Reference: Determination of the residues of BYI08330 in/on plu m after spraying of BYI08330 (100 OD) in the field in Germany, northern France and United Kingdom Author(s), year: Schöning R.; Helfrich P.; 2006 Report/Doc. number: RA-2124/04, including trials no . R 2004 0774/2, R 2004 0775/0, R 2004 0776/9, R 2004 0777/7 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the residues of BYI08330 in/on plu m after spraying of BYI08330 (150 OD) in the field in United Kingdom, n orthern France and Germany Author(s), year: Schöning R.; 2006 Report/Doc. number: RA-2004/05, including trials no . R 2005 0050/5, R 2005 0051/3, R 2005 0052/1, R 2005 0054/8 M-266052-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

### - 64 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Reference: Determination of the residues of BYI08330 in/on plu m after spraying of BYI08330 (100 OD) in the field in southern France a nd Italy Author(s), year: Schöning R.; Wolters A.; 2006 Report/Doc. number: RA-2125/04, including trials no . R 2004 0778/5, R 2004 0779/3 M-262626-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the residues of BYI08330 in/on plu m after spraying of BYI08330 (150 OD) in the field in Italy and Spain Author(s), year: Schöning R.; 2006 Report/Doc. number: RA-2005/05, including trials no . R 2005 0055/6, R 2005 0058/0 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Experimental design: Altogether 12 supervised residue trials were conduc ted in plums in 2004 and 2005. 8 of these trials we re carried out in the Northern European region (German y, UK, N-France) and 4 trials in the South (S-Franc e, Italy and Spain). The studies were carried out usin g oil based dispersion concentrate formulations, containing 150 g/L and 100 g/L of spirotetramat. The product was used two times with an application rate of 0.072 kg a.s./ha and meter height of leaf s urface (2 – 3 m), resulting application rates between 0.14 4 and 0.2160 kg a.s./ha. All trials were performed according to the critical European GAP. An overview on the supervised residue trials is giv en in Table B.7.6.4.2-2. Table B.7.6.4.2-2: Overview on supervised residue trials with BYI08330 in plum

Study no. Region Formulation No. of

trials Year Use rate (g as/ha x m CH) Water

volume (L/ha x m CH) (a) No of

appl. Spray

interval (days) PHI

days

RA-2124/04 N-EU OD 100 4 2004 72 500 2 14 21-28 RA-2004/05 N-EU OD150 4 2005 72 500 2 14 21-28 RA-2125/04 S-EU OD 100 2 2004 72 500 2 14 21

RA-2005/05 S-EU OD150 2 2005 72 500 2 14 21 

### The second application was carried out at BBCH grow th stage 75-81. The plums samples were taken before the last applic ation, 0, 7, 14, 21 and 28 days after the last appl ication. After the harvest the samples were frozen within a maximum of 24 hours after sampling and stored at – 18°C until analysis. Analytical method used in all studies: Residues fruit were analysed according to method 00 857 (see). Residues of spirotetramat and its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-mono-hydroxy and BYI 08330-enol-Glc in peach and apricot were determined by HPLC-ESI-MS/MS according to method 00857. The limit of quantification (LOQ, defined as the lo west validated fortification level) was 0.01 mg/kg for spirotetramat, 0.012 mg/kg for its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and 0.008 mg/kg for BYI 08330-enol-Glc in/o n plums, calculated as spirotetramat equivalent.

### - 65 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

The mean procedural recoveries at the fortification levels of 0.01 to 2.0 mg/kg for spirotetramat and its four metabolites ranged between 88 and 105% and RSD < 20 %; these results indicate that the methods used were suitable for this analysis. Findings: A detailed summary of the residue trial for plums i s given in Annex I e. The total residue of spirotetramat in plums from ei ght residue trials in Northern Europe after two app lications ranged between 0.119 mg/kg and 0.828 mg/kg. As plum s are regarded as minor crops in Southern Europe four residue decline trials were performed. Residue s resulting from these trials ranged between 0.135 mg/kg and 0.485 mg/kg. All residue trials were carried out according the i ntended GAP. The total residue of spirotetramat is composed of m ainly BYI08330 enol (0.023 – 0.32 mg/kg parent equivalents). The parent compound, the ketohydroxy, the monohydroxy and enol-glucoside metabolite generally are minor compounds. In some trials the m onohydroxy metabolite appeared at amounts similar t o the enol metabolite (0.018 to 0.33 mg/kg). An overview of the European residue data for spirot etramat and its metabolites in plums is given in th e table below. Table B.7.6.4.2-3: Overview of European residue dat a for spirotetramat and its metabolites in plums used 2 times with application rates of 0.076 kg a.s ./ha and meter canopy height (residues are calculated as spirotetramat equivalent):

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 Northern Europe plum / OD 100 WurzenRoitzsch, Germany, 2004 fruit

fruit fruit fruit 0

14 21 28 0.20

0.08 0.05 0.04 0.31

0.45 0.32 0.29 0.027

0.041 0.031 0.038 0.086

0.25 0.25 0.33 0.034

0.11 0.10 0.13 0.657

0.931 0.751 0.828 plum / OD 100 Burscheid,

Germany, 2004 fruit

fruit fruit fruit 0

14 21 28 0.16

0.02 0.01 0.01 0.071

0.061 0.034 0.015 0.012

0.012 0.012 0.012 0.031

0.072 0.078 0.084 0.008

0.020 0.025 0.024 0.282

0.185 0.159 0.145 plum / OD 100 Pouligny St.

Pierre, NFrance, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 7 14 21 28 0.08

0.37 0.16 0.09 0.07 0.06 0.21

0.22 0.31 0.25 0.26 0.26 0.027

0.029 0.029 0.025 0.025 0.028 0.049

0.053 0.058 0.057 0.064 0.084 0.05

0.057 0.078 0.078 0.11 0.15 0.416

0.729 0.635 0.5 0.529 0.582 plum / OD 100 Cambridge,

UK, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 7 14 21 28 0.07

0.25 0.14 0.10 0.09 0.07 0.15

0.15 0.17 0.17 0.13 0.14 0.012

0.012 0.012 0.015 0.014 0.017 0.089

0.085 0.11 0.13 0.15 0.20 0.042

0.042 0.046 0.055 0.064 0.084 0.363

0.539 0.478 0.47 0.448 0.511 plum / OD 150 Cambridge,

UK, 2005 fruit

fruit fruit fruit 0

14 21 28 0.16

0.07 0.04 0.03 0.092

0.17 0.19 0.14 0.012

0.012 0.012 0.012 0.017

0.037 0.078 0.083 0.008

0.015 0.033 0.034 0.289

0.304 0.353 0.299 plum / OD 150 Pouligny St.

Pierre, France, 2005 fruit

fruit fruit fruit 0

14 21 28 0.26

0.06 0.04 0.03 0.09

0.099 0.11 0.063 0.012

0.012 0.012 0.012 0.096

0.21 0.23 0.19 0.011

0.019 0.024 0.016 0.469

0.400 0.416 0.311

### - 66 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 plum / OD 150 Monheim,

Germany, 2005 fruit

fruit fruit fruit fruit fruit 0*

0 7 14 21 28 0.01

0.08 0.05 0.03 0.02 0.02 0.023

0.044 0.095 0.062 0.027 0.043 0.012

0.012 0.017 0.015 0.017 0.012 0.012

0.012 0.062 0.11 0.098 0.10 <0.008

<0.008 0.009 0.016 0.016 0.018 0.065

0.156 0.233 0.233 0.178 0.193 plum / OD 150 WurzenRoitzsch, Germany, 2005 fruit

fruit fruit fruit fruit fruit 0*

0 7 14 21 28 0.02

0.08 0.06 0.05 0.02 0.03 0.039

0.052 0.082 0.074 0.041 0.043 0.012

0.012 0.012 0.012 0.012 0.012 0.014

0.017 0.019 0.021 0.018 0.022 0.008

0.008 0.010 0.009 0.010 0.012 0.093

0.169 0.183 0.166 0.101 0.119 Southern Europe plum / OD 100 Fronton, SFrance, 2004 fruit

fruit fruit fruit 0

14 21 28 0.15

0.09 0.06 0.05 0.12

0.19 0.16 0.11 0.013

0.021 0.021 0.02 0.073

0.19 0.2 0.22 0.022

0.043 0.044 0.044 0.378

0.534 0.485 0.444 plum / OD 100 Ravenna,

Italy, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 7 14 21 28 0.03

0.21 0.11 0.04 0.03 0.02 0.093

0.096 0.18 0.15 0.092 0.06 0.014

0.018 0.018 0.016 0.013 0.012 0.012

0.012 0.014 0.02 0.023 0.029 0.009

0.009 0.014 0.021 0.023 0.028 0.158

0.345 0.336 0.247 0.181 0.149 plum / OD 150 Viglona,

Italy, 2005 fruit

fruit fruit fruit 0

14 21 28 0.34

0.09 0.08 0.03 0.055

0.12 0.088 0.037 0.012

0.012 0.012 0.012 0.054

0.13 0.17 0.15 0.018

0.04 0.045 0.036 0.479

0.392 0.395 0.265 plum / OD 150 Pobla del

Duc, Spain, 2005 fruit

fruit fruit fruit fruit fruit 0*

0 7 14 21 28 0.03

0.12 0.11 0.07 0.05 0.03 0.036

0.047 0.063 0.054 0.044 0.025 0.012

0.012 0.012 0.012 0.012 0.012 0.012

0.012 0.012 0.018 0.021 0.021 <0.008

0.008 0.008 0.008 0.008 0.009 0.09

0.199 0.205 0.162 0.135 0.097



### For the calculation of the MRL proposal, both of th e prescribed methods I and II have been used for spirotetramat in plums (based on data obtained from trials from Northern and Southern Europe):

MRL-calculation based on data obtained from the Nor thern Region: Individual data points for plum are: 0.119 mg/kg, 0.145 mg/kg, 0.193 mg/kg, 0.353 mg/kg, 0.416 mg/kg, 0.511 mg/kg, 0.582 mg/kg, 0.828 mg/kg

, Mean residue: 0.393 mg/kg; standard deviation: 0.24 4 mg/kg STMR: 0.38 mg/kg Highest residue: 0.828 mg/kg Method I: R max 

### = 1.172 mg/kg Method II: R ber 

### = 1.129 mg/kg Based on the data available for plum in Northern Eu rope, a MRL of 2 mg/kg can be proposed.

MRL-calculation based on data obtained from the Sou thern Region: Individual data points for plum are: 0.135 mg/kg, 0.181 mg/kg, 0.395 mg/kg, 0.485 mg/kg, Mean residue: 0.299 mg/kg; standard deviation: 0.16 8 mg/kg STMR: 0.29 mg/kg Highest residue: 0.485 mg/kg

### - 67 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Method I: R max 

### = 1.163 mg/kg Method II: R ber 

### = 0.9250 mg/kg Based on the data available for plum in Southern Eu rope, a MRL of 2 mg/kg can be proposed. Conclusion: During 2004 and 2005 altogether 12 residue trials w ere carried out on plums in North and South Europe according to the intended GAP. The trials were cond ucted using BYI 08330 OD 100 and BYI 08330 OD 150 as formulations. The residues in plums were similar and resulted in a MRL of 2 mg/kg of spirotetramat and its metabolites. The highest residue in N-EU reached 0. 828 mg/kg whereas in S-EU 0.485 mg/kg were found. Comments (RMS): No comments.

B.7.6.4.3 Cherry

Spirotetramat is supported for control of aphids, s cales, and mites in peaches and apricots. The criti cal European GAP for the use in northern (N-EU) and sou thern Europe (S-EU) is summarized in Table B.7.6.4.3-1. Table B.7.6.4.3-1: GAP for residue situation in che rry North or South of EU Indoor or

outdoor Number of

applications Mode of

application Growth stage at

last application Application rate expressed

under the relevant unit PHI (d) EU-N F 2 Spray BBCH 81 0.072 kg a.s./ha and m canopy height, max. 0.216 kg a.s./ha 21

EU-S F 2 Spray BBCH 81 0.072 kg a.s./ha and m canopy height, max. 0.216 kg a.s./ha 21



### Reference: Determination of the residues of BYI08330 in/on swe et cherry and sour cherry after spraying of BYI08330 (100 OD) in the f ield in northern France and Germany Author(s), year: Schöning R.; Behn, U. ; Wolters A. ; 2006 Report/Doc. number: RA-2119/04, including trials no . R 2004 0718/1, R 2004 0720/3, R 2004 0721/1, R 2004 0723/8 M-263879-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the residues of BYI08330 in/on swe et cherry and sour cherry after spraying of BYI08330 (150 OD) in the f ield in Germany and northern France Author(s), year: Schöning R.; Raecker T.; 2006 Report/Doc. number: RA-2008/05, including trials no . R 2005 0068/8, R 2005 0071/8, R 2005 0072/6 M-267524-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

### - 68 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Reference: Determination of the residues of BYI08330 in/on swe et cherry after spraying of BYI08330 (100 OD) in the field in Italy and sout hern France Author(s), year: Schöning R.; Wolters A.; 2005 Report/Doc. number: RA-2118/04, including trials no . R 2004 0716/5, R 2004 0717/3 M-260405-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the residues of BYI08330 in/on swe et cherry after spraying of BYI08330 (150 OD) in the field in Italy and Spai n Author(s), year: Schöning R.; Eberhardt R.; 2006 Report/Doc. number: RA-2009/05, including trials no . R 2005 0073/4, R 2005 0074/2 M-267488-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Experimental design Spirotetramat is intended for use on sweet and sour cherries in Northern and Southern European regions

. All studies were carried out in 2004 and 2005 using oil based dispersion concentrates containing 150 g /L and 100 g/L of spirotetramat. For northern Europe 4 residue trials (Germany and N -France) on sweet cherries and three trials on sour cherries were conducted. In southern Europe 4 residue trials on sweet cherri es were performed in Italy, Spain and S-France. According to guidance document SANCO 7525/VI/95/rev .7, cherries are regarded as minor crops in Europe, but for extrapolation four trials of each are neces sary to extrapolate to the group cherry. The product was used twice with an application rate of 0.072 kg a.s./ha and meter height of leaf surfa ce (2 – 3 m), resulting application rates between 0.144 and 0.2160 kg a.s./ha. All trials were performed accor ding to the critical European GAP. The second application was carried out at BBCH grow th stage 75-85. All residue trials were conducted as residue declin e studies. The specimens were taken before the last application, 0, 7, 14, 21 and 28 days after the las t application. All samples were stored deep frozen within 24 hours after sampling. The time intervals between date of deep-freezing and the last extraction ranged from 7 6 to 211 days. Analytical method used in all studies: Residues fruit were analysed according to method 00 857 (see IIA Point 4.3.1). Mean concurrent recoveri es Residues of spirotetramat and its metabolites BYI 0 8330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and BYI 08330-enol-Glc in peach and apricot were determined by HPLC-ESI-MS/MS according to method 00857. The limit of quantification (LOQ, defined as the lowest validated fortificatio n level) was 0.01 mg/kg for spirotetramat, 0.012 mg/kg for its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and 0.008 mg/kg for BYI 08330-enol-Glc in/o n cherries, calculated as spirotetramat equivalent. The mean procedural recoveries at the fortification levels of 0.01 to 1.0 mg/kg f or spirotetramat and its four metabolites ranged between 85 and 96 % and RSD < 20 %; these results indicate that the methods used were suitable for this analysis.

### - 69 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Findings: A detailed summary of the residue trial for cherrie s is given in Annex If. The total residue of spirotetramat in cherries from seven residue trials in Northern Europe after two applications ranged between 0.248 mg/kg and 0.939 m g/kg. Residues resulting from residue trials from Southern Europe ranged between 0.629 mg/kg and 1.04 5 mg/kg. All residue trials were carried out according the i ntended GAP. Control samples were performed at each location. In one control sample from a study in Northern Europe (RA-209/05) a total residue of total spirotetramat was found at 0.55 mg/kg. The value was confirmed by the analysis of the retained sample, but no further exp lanation was given. Major component of the total residue of spirotetram at in all trials was the enol metabolite. All other components were present at lower amounts. In cherri es from some trials the monohydroxy metabolite coul d be detected at similar amounts as the enol metaboli te. An overview of the European residue data for spirot etramat and its metabolites is given in the table b elow. Table B.7.6.4.3-2: Overview of European residue dat a for spirotetramat and its metabolites in cherries used 2 times with application rates of 0.076 kg a.s ./ha and meter canopy height (residues are calculated as spirotetramat equivalent):

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 Northern Europe

sweet cherry / OD 100 Pouligny

SaintPierre, NFrance, 2004 fruit

fruit fruit fruit fruit 0*

0 14 21 28 0.09

0.43 0.02 0.01 0.01 0.15

0.25 0.32 0.32 0.23 0.18

0.21 0.19 0.11 0.089 0.024

0.026 0.081 0.12 0.13 0.008

0.008 0.018 0.023 0.026 0.452

0.924 0.629 0.583 0.485 sour cherry / OD 100 Wurzen

Roitzsch, Germany, 2004 fruit

fruit fruit fruit fruit 0*

0 14 21 28 0.12

0.56 0.03 0.01 0.01 0.20

0.25 0.25 0.21 0.12 0.10

0.10 0.06 0.033 0.024 0.018

0.017 0.021 0.021 0.022 0.017

0.014 0.013 0.011 0.013 0.455

0.941 0.374 0.285 0.189

sweet cherry / OD 100 Brain sur

L’Authion, N-France, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 7 13 21 27 0.03

0.39 0.03 0.03 0.02 0.01 0.70

0.63 0.79 0.86 0.58 0.39 0.11

0.098 0.087 0.11 0.072 0.055 0.069

0.057 0.093 0.17 0.17 0.11 0.054

0.047 0.057 0.11 0.097 0.065 0.963

1.222 1.057 1.280 0.939 0.630 sour cherry / OD 100 Burscheid,

Germany, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 7 14 21 28 0.01

0.51 0.02 0.01 0.01 <0.01 0.099

0.17 0.41 0.29 0.21 0.13 0.013

0.014 0.018 0.016 0.012 0.012 0.012

0.012 0.019 0.030 0.040 0.041 0.008

0.008 0.011 0.016 0.023 0.020 0.142

0.714 0.478 0.362 0.295 0.213

sweet cherry / OD 150 Wurzen

Roitzsch, Germany, 2005 fruit

fruit fruit 0

14 21 0.69

0.03 0.02 0.26

0.53 0.36 0.052

0.13 0.13 0.074

0.17 0.23 0.018

0.057 0.086 1.094

0.917 0.826

sweet cherry / OD 150 Pouligny

SaintPierre, NFrance, 2005 fruit

fruit fruit fruit fruit fruit 0*

0 7 14 21 28 0.03

0.28 0.04 0.02 0.01 0.01 0.092

0.27 0.44 0.31 0.23 0.19 0.072

0.090 0.12 0.082 0.068 0.067 0.012

0.012 0.049 0.059 0.091 0.21 0.008

0.008 0.011 0.013 0.018 0.047 0.214

0.660 0.660 0.484 0.417 0.524

### - 70 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 sour cherry / OD 150 Monheim,

Germany, 2005 fruit

fruit fruit fruit fruit fruit 0*

0 7 14 21 28 0.02

0.31 0.10 0.02 <0.01 <0.01 0.041

0.13 0.30 0.29 0.15 0.093 0.035

0.030 0.046 0.040 0.022 0.015 0.012

0.012 0.033 0.054 0.037 0.038 0.008

0.008 0.024 0.039 0.029 0.028 0.116

0.49 0.503 0.443 0.248 0.184 Southern Europe

sweet cherry / OD 100 Bisceglie,

Italy, 2004 fruit

fruit fruit fruit fruit 0*

0 14 21 28 0.04

0.25 0.04 0.01 <0.01 0.18

0.22 0.48 0.38 0.24 0.22

0.23 0.19 0.11 0.085 0.029

0.027 0.067 0.11 0.10 0.008

0.008 0.018 0.019 0.019 0.477

0.735 0.795 0.629 0.454

sweet cherry / OD 100 Monteux, SFrance, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 9 14 21 28 0.05

0.43 0.07 0.06 0.05 0.02 0.18

0.28 0.52 0.50 0.50 0.35 0.12

0.12 0.14 0.11 0.11 0.086 0.024

0.022 0.11 0.21 0.32 0.37 0.008

0.008 0.021 0.038 0.065 0.071 0.382

0.86 0.861 0.918 1.045 0.897

sweet cherry / OD 150 Andria,

Italy, 2005 fruit

fruit fruit fruit 0

14 21 28 0.29

0.02 0.01 0.01 0.77

0.57 0.35 0.26 0.093

0.099 0.055 0.044 0.54

0.39 0.22 0.14 0.11

0.073 0.044 0.027 1.803

1.152 0.679 0.481

sweet cherry / OD 150 Santa

Coloma de Cervelló, Spain, 2005 fruit

fruit fruit fruit fruit fruit 0*

0 7 14 21 28 0.01

0.34 0.12 0.09 0.06 0.05 0.29

0.41 0.47 0.32 0.22 0.10 0.072

0.072 0.076 0.075 0.073 0.076 0.083

0.092 0.20 0.30 0.29 0.33 0.017

0.019 0.042 0.069 0.078 0.095 0.472

0.933 0.908 0.854 0.721 0.651



### According to the guidance document SANCO 7525/VI/95 /rev. 7, cherries are regarded as minor crops in Europe and an extrapolation to the group cherry is possible from sweet and sour cherry with four trial s each. Although only three residue trials on sour cherry w ere submitted all results of sweet and sour cherrie s were taken for the calculation of the MRL proposal for N orthern Europe. For the Southern European region no extrapolation is possible according the above menti oned guidance paper. For MRL calculation, both of the prescribed methods I and II have been used for spirotetramat in cherr ies (based on data obtained from trials from Southern E urope):

MRL-calculation based on data obtained from the Nor thern Region: Individual data points for sweet cherry are: 0.524 mg/kg, 0.583 mg/kg, 0.826 mg/kg, 0.939 mg/kg, Individual data points for sour cherry are: 0.248 mg/kg, 0.285 mg/kg, 0.295 mg/kg Mean residue: 0.829 mg/kg; standard deviation: 0.27 5 mg/kg STMR: 0.52 mg/kg Highest residue: 0.939 mg/kg Method I: R max 

### = 1.463 mg/kg Method II: R ber 

### = 1.652 mg/kg Based on the data available for cherries, a MRL of 2 mg/kg can be proposed.

MRL-calculation based on data obtained from the Sou thern Region: Individual data points for sweet cherries are: 0.629 mg/kg, 0.679 mg/kg, 0.721 mg/kg, 1.045 mg/kg

### - 71 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Mean residue: 0.769mg/kg; standard deviation: 0.18 8 mg/kg STMR: 0.70 mg/kg; Highest residue: 1.045 mg/kg Method I: R max 

### = 1.736 mg/kg Method II: R ber 

### = 1.928 mg/kg Based on the data available for cherries, a MRL of 2 mg/kg can be proposed. Conclusion: In 2004 and 2005, altogether 13 residue trials were conducted on sweet and sour cherries in Northern a nd Southern Europe using two different formulations of spirotetramat (OD 100 and OD 150). All trials were performed according to the intended European GAP. For Northern Europe 4 trials on sweet cherries and 3 trials on sour cherries were submitted and 4 tria ls on sweet cherries from Southern Europe. The residues in sweet and sour cherries from Northe rn and Southern Europe resulted in the MRL of 2 mg/ kg. The highest residue was reached in Southern Europe with 1.045 mg/kg. Comments (RMS): No comments.

B.7.6.5 Berries and small fruits

B.7.6.5.1 Grapes

Spirotetramat is applied for the use in grapes for the control of mealy bugs and phylloxer. The critic al European GAP for the use in Northern (N-EU) and Sou thern Europe (S-EU) is summarized in Table B.7.6.5.1-1: Table B.7.6.5.1-1: GAP for residue situation in gr apes North or South of EU Indoor or

outdoor Number of

applications Mode of

application Growth stage at

last application Application rate expressed

under the relevant unit PHI (d) EU-N F 2 Spray BBCH 82 0.072 kg a.s./ha 14 EU-S F 2 Spray BBCH 82 0.096 kg a.s./ha 14



### Reference: Determination of the residues of BYI08330 in/on gra pe and table grape after spraying and low–volume spraying of BYI08330 (100 O D) in the field in Italy, Greece, Spain and southern France Author(s), year: Schöning R.; Eberhardt R.; 2006 Report/Doc. number: RA-2049/04, including trials no . R 2004 0196/5, R 2004 0197/3, R 2004 0198/1, R 2004 0201/5, R 2004 0202/3, R 2004 0203/1 M-263864-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

### - 72 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Reference: Determination of the residues of BYI08330 in/on gra pe after spraying of BYI08330 (150 OD) in the field in Spain and Italy Author(s), year: Ballesteros C.; Gateaud L.; 2006 Report/Doc. number: RA-2034/05, including trials no . R 2005 0157/9, R 2005 0158/7 M-270088-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the residues of BYI08330 in/on gra pe after spraying of BYI08330 (48 SC) in the field in France and Italy Author(s), year: Ballesteros C.; Gateaud L.; 2006 Report/Doc. number: RA-2036/05, including trials no . R 2005 0161/7, R 2005 0162/5 M-273708-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Experimental design: During 2004 and 2005 10 supervised residue trials o n grapes were performed according to the intended GAP in Southern Europe (Italy, Greece, Spain and S/ France). The studies were carried out using oil bas ed dispersion concentrate formulations, containing 150 g/L and 100 g/L of spirotetramat and one study was conducted with a suspension concentrate with 48 g s pirotetramat/L. For northern Europe, no trials were performed. The product was used two times with an application rate of 0.096 kg a.s./ha. To cover the different agricultural practices of different European countr ies spray applications were conducted using a water volume of 160 to 1500 L water/ha. An overview on th e supervised residue trials is given in Table B.7.6 .5.1-2. Table B.7.6.5.1-2: Overview on supervised residue t rials with spirotetramat in grapes

Study no. Region Formula tion No. of

trials Year Use rate

(g as/ha) Water

volume (L/ha) No of

appl. Spray interval (days) PHI

days

RA-2049/04 S-EU OD 100 6 2004 96 1500 2 14 14 RA-2034/05 S-EU OD 150 2 2005 96 800, 1000 2 14 14 RA-2036/05 S-EU SC 048 2 2005 96 160, 1000 2 14 14 

### The second application was carried out at BBCH grow th stage 75-85. The samples were taken before the last application, 0, 7, 14, 21 and 28 days after the last applicatio n. After the harvest the samples were frozen within a maximum of 24 hours after sampling and stored at – 18°C until analysis. Samples bunch of grapes were taken before the last application, 0, 3, 7, 14 and 21 days after the last application. The samples of the berries of grapes w ere taken at 7, 14 and 21 days after application. All samples were stored deep frozen within 24 hours after sampling. The time intervals between date of deep-freezing and the last extraction ranged from 4 7 to 249 days.

Analytical method used in all studies: Residues of spirotetramat and its metabolites BYI 0 8330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and BYI 08330-enol-Glc in the berries and b unch of the grapes were determined by HPLC-ESIMS/MS according to method 00857.

### - 73 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

The limit of quantification (LOQ, defined as the lowest validated fortificatio n level) was 0.01 mg/kg for spirotetramat, 0.012 mg/kg for its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and 0.008 mg/kg for BYI 08330-enol-Glc in/o n grapes (bunch and berries), calculated as spirotetramat equivalent. The mean procedural recoveries at the fortification levels of 0.01 to 2.0 mg/kg f or spirotetramat and its four metabolites ranged between 85 and 104% and RSD < 20 %; these results indicate that the methods used were suitable for this analysis. Findings: A detailed summary of the residue trial for citrus fruits is given in Annex I g. The total residue of spirotetramat in bunch of grap es ranged between 0.118 and 0.537 mg/kg (STMR 0.266 mg/kg). The total residue in berries ranged between 0.167 to 0.641 mg/kg (STMR 0.272 mg/kg) and did no t differ significantly from the residue in bunch of g rapes. There was no difference in residues after spraying of different water rates per ha. Moreover an influe nce of different formulations of spirotetramat (OD100, OD1 50 of SC048) was not detected. Major component of the total residue of spirotetram at in bunch of grapes and berries from all trials s ampled at the PHI of 14 days after two spray applications was the parent compound. In many trials the enol metabolite was detected at similar amounts. BYI0833 0-ketohydroxy and enol-glucoside were minor metabolites, BYI08330-monohydroxy was not detected or in traces, only. An overview of the European residue data for spirot etramat and its metabolites is given in the table b elow.

Table B.7.6.5.1-3: Overview of European residue dat a for spirotetramat and its metabolites in grapes used 2 times with application rates of 0.096 kg a.s ./ha (residues are calculated as spirotetramat equivalent):

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 Southern Europe grape / OD 100 Bologna,

Italy, 2004 bunch

bunch bunch bunch berry bunch berry bunch berry 0*

0 3 7 7 14 14 21 21 0.03

0.37 0.14 0.15 0.14 0.17 0.12 0.12 0.08 0.040

0.10 0.11 0.17 0.15 0.095 0.092 0.059 0.041 0.060

0.078 0.047 0.095 0.085 0.10 0.072 0.074 0.060 0.012

0.012 0.012 0.012 0.012 0.012 0.012 0.012 0.012 0.041

0.042 0.031 0.11 0.10 0.16 0.18 0.16 0.16 0.183

0.602 0.340 0.537 0.487 0.537 0.476 0.425 0.353 grape / OD 100 San

Prospero, Italy, 2004 bunch

bunch bunch berry bunch berry bunch berry 0*

0 7 7 14 14 21 21 0.14

0.20 0.20 0.17 0.03 0.06 0.03 0.03 0.030

0.042 0.045 0.037 0.022 0.035 0.022 0.022 0.025

0.027 0.045 0.031 0.020 0.038 0.024 0.020 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.020

0.018 0.026 0.026 0.019 0.038 0.030 0.030 0.227

0.299 0.328 0.276 0.103 0.183 0.118 0.114

### - 74 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 table grape / OD 100 Korinthos,

Greece, 2004 bunch

berry bunch berry bunch berry bunch berry bunch berry bunch berry 0*

0* 0 0 3 3 7 7 14 14 21 21 0.05

0.05 0.17 0.14 0.15 0.12 0.15 0.16 0.08 0.08 0.10 0.08 0.064

0.066 0.092 0.089 0.096 0.081 0.11 0.11 0.11 0.11 0.11 0.11 0.012

0.012 0.015 0.012 0.015 0.013 0.018 0.018 0.012 0.013 0.016 0.014 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.022

0.023 0.023 0.025 0.027 0.025 0.033 0.037 0.043 0.045 0.054 0.051 0.16

0.163 0.312 0.278 0.300 0.251 0.323 0.337 0.257 0.260 0.292 0.267 table grape / OD 100 Cieza,

Spain, 2004 bunch

berry bunch berry bunch berry bunch berry bunch berry bunch berry 0*

0* 0 0 3 3 7 7 15 15 21 21 0.22

0.22 0.32 0.52 0.45 0.49 0.37 0.30 0.20 0.47 0.21 0.33 0.030

0.031 0.035 0.050 0.044 0.040 0.039 0.027 0.021 0.047 0.018 0.031 0.033

0.032 0.022 0.034 0.049 0.050 0.040 0.025 0.024 0.054 0.021 0.035 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.028

0.028 0.017 0.027 0.033 0.031 0.029 0.022 0.027 0.058 0.030 0.054 0.323

0.323 0.406 0.643 0.588 0.623 0.490 0.386 0.284 0.641 0.291 0.462 table grape / OD 100 Vacquiers,

S-France, 2004 bunch

berry bunch berry bunch berry bunch berry bunch berry 0*

0* 0 0 7 7 14 14 21 21 0.07

0.06 0.19 0.18 0.10 0.09 0.11 0.13 0.09 0.09 0.033

0.030 0.041 0.034 0.037 0.032 0.044 0.055 0.040 0.038 0.012

0.012 0.012 0.012 0.012 0.012 0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.012 <0.012 <0.012 0.023

0.020 0.024 0.024 0.032 0.033 0.063 0.074 0.062 0.063 0.15

0.134 0.279 0.262 0.193 0.179 0.241 0.283 0.216 0.215 table grape / OD 100 Anchialos,

Greece, 2004 bunch

berry bunch berry bunch berry bunch berry bunch berry 0*

0* 0 0 7 7 14 14 21 21 0.03

0.10 0.14 0.09 0.15 0.11 0.05 0.15 0.05 0.02 0.024

0.043 0.023 0.043 0.057 0.045 0.042 0.022 0.034 0.022 0.012

0.020 0.012 0.017 0.018 0.014 0.012 0.012 0.013 0.012 <0.012

0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.028

0.093 0.027 0.082 0.060 0.036 0.040 0.022 0.043 0.031 0.106

0.268 0.214 0.244 0.297 0.217 0.156 0.218 0.152 0.097 grape / OD 150 Campo

Arcis, Spain, 2005 bunch

bunch bunch bunch berry bunch berry bunch berry 0*

0 3 7 7 14 14 21 21 0.09

0.39 0.32 0.09 0.11 0.09 0.07 0.07 0.06 0.029

0.038 0.030 0.030 0.034 0.027 0.031 0.022 0.024 0.013

<0.012 0.014 0.017 0.014 0.019 0.019 0.018 0.019 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.015

0.011 0.013 0.017 0.022 0.031 0.035 0.029 0.030 0.159

0.463 0.389 0.166 0.192 0.179 0.167 0.151 0.145

### - 75 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 grape / OD 150 Bologna,

Italy, 2005 bunch

bunch bunch bunch berry bunch berry bunch berry 0*

0 3 7 7 14 14 21 21 0.14

0.34 0.19 0.11 0.19 0.13 0.16 0.05 0.03 0.062

0.057 0.12 0.22 0.20 0.17 0.21 0.14 0.12 0.027

0.022 0.026 0.028 0.040 0.035 0.041 0.034 0.029 <0.012

<0.012 <0.012 0.014 0.016 <0.012 <0.012 0.014 <0.012 0.040

0.036 0.039 0.082 0.11 0.13 0.15 0.15 0.15 0.281

0.467 0.387 0.454 0.556 0.477 0.573 0.388 0.341 grape / 048 SC Vendeuvre

du Poitou, S-France, 2005 bunch

bunch berry bunch berry bunch berry 0

7 7 14 14 21 21 0.21

0.20 0.14 0.17 0.16 0.14 0.12 <0.012

0.012 <0.012 0.015 <0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 0.009 0.011 0.008 0.015 0.017 0.254

0.244 0.185 0.22 0.204 0.191 0.173 grape / 048 SC Bologna,

Italy, 2005 bunch

bunch berry bunch berry bunch berry 0

7 7 14 14 21 21 0.11

0.08 0.08 0.10 0.07 0.03 0.03 0.027

0.13 0.14 0.14 0.15 0.099 0.10 <0.012

0.019 0.015 0.026 0.021 0.018 0.018 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.014

0.052 0.063 0.084 0.095 0.11 0.11 0.175

0.293 0.31 0.362 0.348 0.269 0.270



### Residues in berries were used for the estimation of the dietary risk and for MRL setting. For the calculation of the MRL proposal, both of th e prescribed methods I and II have been used for spirotetramat in grapes (based on data obtained fro m trials from Southern Europe):

MRL-calculation based on data obtained from the Sou thern Region: Individual data points for grapes are: 0.167 mg/kg, 0.183 mg/kg, 0.204 mg/kg, 0.218 mg/kg, 0.26 mg/kg, 0.283 mg/kg, 0.348 mg/kg, 0.476 mg/kg, 0.573 mg/kg, 0.641 mg/kg Mean residue: 0.335 mg/kg; standard deviation: 0.01 7 mg/kg STMR: 0.272 mg/kg Highest residue: 0.641 mg/kg Method I: R max 

### = 0.831 mg/kg Method II: R ber 

### = 1.001 mg/kg Based on the data available for grapes, a MRL of 1 mg/kg can be proposed. Conclusion: During 2004 and 2005 altogether 10 residue trials w ere carried out on grapes in Southern Europe accord ing to the intended GAP. The trials were conducted usin g BYI 08330 OD 100, BYI 08330 OD 150 and BYI 08330 048 SC as formulations. The residues in grapes were comparable and resulted in a MRL of 1 mg/kg of spirotetramat and its metabolites. The highest resi due in S-EU reached 0.641 mg/kg. No residue trials for Northern Europe were submitte d. Therefore the evaluation of the residue situatio n in grapes is limited to South-Europe and the MRL is ba sed on S-EU data only. Comments (RMS): No comments.

B.7.6.5.2 Strawberry

Spirotetramat is applied for control of aphids and white flies in strawberries. The critical European GAP for the use in northern (N-EU) and southern Europe (S-E U) is summarized in Table B.7.6.5.2-1.

### - 76 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.6.5.2-1: GAP for residue situation in st rawberries

North or South of EU Indoor or

outdoor Number of

applications Mode of

application Growth stage at

last application Application rate expressed

under the relevant unit PHI (d) EU-N F 2 Spray BBCH 87 0.096 g a.s./ha 3 EU-S F 2 Spray BBCH 87 0.096 g a.s./ha 3 EU-N/S G 2 Spray BBCH 87 0.096 g a.s./ha 3



### Reference: Determination of the Residues of BYI08330 in/on Str awberry after Spraying of BYI08330 (100 OD) in the Greenhouse in Germany a nd France Author(s), year: Freitag T.; Eberhardt R.; 2006 Report/Doc. number: RA-2122/04, including trials no . R 2004 0726/2, R 2004 0765/3, R 2004 0766/1, R 2004 0768/8, R 2004 0769/6, R 2004 0771/8, R 2004 0 772/6, R 2004 0773/4 M-263736-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the Residues of BYI08330 in/on Str awberry after Spraying of BYI08330 (100 OD) in the Field in Germany and No rthern France Author(s), year: Freitag T.; Helfrich P.; 2006 ; am ended 18.01.2006 Report/Doc. number: RA-2120/04, including trials no. R 2004 0724/6, R 2004 0759/9, R 2004 0760/2, R 2004 0761/0 M-262423-02-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the Residues of BYI08330 in/on Str awberry after Spraying of BYI08330 (100 OD) in the Field in Italy, Spain and Southern France Author(s), year: Freitag T.; Helfrich P.; 2006 Report/Doc. number: RA-2121/04, including trials no . R 2004 0725/4, R 2004 0762/9, R 2004 0763/7, R 2004 0764/5 M-262418-02-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Experimental design: The magnitude of residues of spirotetramat and its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-mono-hydroxy and BYI 08330-enol-Glc in/on str awberries harvested following the treatment with BY I 08330 100 OD formulation in greenhouse (Germany and France,) and under field conditions (N-EU: Germany and N-France; S-EU: Italy, Spain and S-Fran ce) was determined. Overall 16 residue trials on strawberry were conduc ted in 2004. An overview on the supervised residue trials conducted with BYI 08330 100 OD formulation is give n in Table B.7.6.5.2-2

### - 77 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.6.5.2-2: Overview on European residue tr ials with BYI08330 in strawberry

Location Formulation No. of trials Year Use rate

(g as/ha) Water volume No of appl. Spray interval

(days)

Greenhouse OD 100 8 2004 96 600-1000 2 14 Field N-EU OD 100 4 2004 96 600-1000 2 14 Field S-EU OD 100 4 2004 96 600-800 2 14 

### All trials were applied according to the intended E uropean GAP. The last application was carried out a t growth stage BBCH 81 - 89. The specimens were taken before the last treatment, 0, 1, 3 and 7 and 14-15 days after the last application. All samples were stored deep frozen within 24 hours after sampling. The time intervals between date of deep-freezing and the last extraction ranged from 1 07 to 365 days. Analytical method used in all studies: Residues of spirotetramat and its metabolites BYI 0 8330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and BYI 08330-enol-Glc in strawberries were determined by HPLC-ESI-MS/MS according to method

00857. The limit of quantification (LOQ, defined as the lo west validated fortification level) was 0.01 mg/kg for spirotetramat, 0.012 mg/kg for its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and 0.008 mg/kg for BYI 08330-enol-Glc in/o n strawberries, calculated as spirotetramat equival ent. The mean procedural recoveries at the fortification levels of 0.01 to 1.0 mg/kg for spirotetramat and its four metabolites ranged between 91 and 96% and RSD < 20% ; these results indicate that the methods used were suitable for this analysis.

Findings: A detailed summary of the residue results is given in Appendix I h. The total residue of spirotetramat in strawberries grown in the greenhouse according to the European G AP ranged between 0.205 and 0.328 mg/kg. In strawberry fruit from 4 field trials in northern Europe a tot al residue of 0.162 to 0.258 mg/kg was detected, in st rawberry fruit from 4 field trials in southern Euro pe a total residue of 0.113 to 0.152 mg/kg was measured. The r esults indicated that the residue level in strawber ries grown in greenhouse is higher than in the field tri als. Therefore, for estimation of the dietary risk and for MRL setting the residue results from the 8 greenhouse r esidue trials were taken in consideration. The residue data used for the evaluation are marked in bold. Major component of the total residue of spirotetram at in strawberries from all trials collected at the PHI of 3 days was BYI08330-enol. The parent compound, the ke tohydroxy and the enol-glucoside were minor components. BYI08330-monohydroxy was not found or i n traces, only.

Table B.7.6.5.2-3: Overview of European residue dat a for spirotetramat and its metabolites in strawberry used 2-3 times with application rates of 0.076 kg a.s./ha (residues are calculated as spirotetramat equivalent):

crop Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330

Greenhouse trials strawberry Bocholt,

Germany, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 7 14 0.01

0.04 0.03 0.01 0.01 0.01 0.13

0.16 0.19 0.19 0.24 0.18 0.012

0.014 0.013 0.012 0.012 0.015 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.008

0.008 0.008 0.008 0.008 0.011 0.172

0.234 0.253 0.232 0.282 0.228

### - 78 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 strawberry Bocholt,

Germany, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 7 14 0.01

0.04 0.01 0.01 0.01 0.01 0.16

0.22 0.13 0.16 0.15 0.14 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 0.012 0.018

0.022 0.014 0.011 0.010 0.019 0.212

0.306 0.178 0.205 0.194 0.193strawberry BornheimSechtem, Germany fruit

fruit fruit fruit fruit fruit 0*

0 1 3 7 14 0.01

0.08 0.06 0.04 0.03 0.02 0.062

0.11 0.15 0.16 0.16 0.071 0.012

0.013 0.014 0.014 0.016 0.014 <0.012

<0.012 <0.012 <0.012 0.012 0.012 0.008

0.009 0.009 0.013 0.026 0.030 0.104

0.224 0.245 0.239 0.244 0.147 strawberry Reynies,

France, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 7 14 0.01

0.04 0.02 0.02 0.01 0.01 0.12

0.14 0.14 0.22 0.28 0.27 0.012

0.012 0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 0.012 0.008

0.008 0.008 0.013 0.014 0.021 0.162

0.212 0.192 0.277 0.328 0.325strawberry TelgteWestbevern, Germany, 2004 fruit

fruit fruit fruit fruit 0*

0 1 3 7 0.03

0.12 0.04 0.03 0.05 0.11

0.16 0.16 0.11 0.21 0.012

0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 0.008

0.008 0.008 0.008 0.008 0.172

0.312 0.232 0.172 0.292strawberry TelgteWestbevern, Germany, 2004 fruit

fruit fruit fruit fruit 0*

0 1 3 7 0.02

0.11 0.06 0.04 0.03 0.075

0.14 0.18 0.16 0.13 0.012

0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 0.008

0.009 0.009 0.010 0.009 0.127

0.283 0.273 0.234 0.193strawberry VechtaLangförden, Germany, 2004 fruit

fruit fruit fruit fruit 0*

0 1 3 7 0.04

0.13 0.11 0.08 0.08 0.15

0.18 0.21 0.17 0.14 0.012

0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 0.008

0.008 0.008 0.008 0.008 0.222

0.342 0.352 0.282 0.252 strawberry Carpentras,

France, 2004 fruit

fruit fruit fruit fruit 0*

0 1 3 7 0.01

0.03 0.02 0.02 0.02 0.18

0.22 0.23 0.25 0.21 0.012

0.013 0.013 0.013 0.013 0.012

0.012 0.012 0.012 0.012 0.008

0.008 0.008 0.008 0.009 0.222

0.283 0.283 0.303 0.264 Field trial – Northern Europe strawberry Bocholt,

Germany, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 7 14 0.01

0.01 0.01 0.01 0.01 <0.01 0.14

0.064 0.084 0.12 0.14 0.060 0.012

0.012 0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.008

0.008 0.008 0.008 0.008 0.008 0.182

0.106 0.126 0.162 0.182 0.102strawberry TelgteWestbevern, Germany, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 7 14 <0.01

0.02 0.01 0.01 0.01 <0.01 0.039

0.033 0.050 0.088 0.12 0.049 0.012

0.012 0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.008

0.008 0.008 0.008 0.008 0.008 0.081

0.085 0.092 0.130 0.162 0.091strawberry Cremery, NFrance, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 7 14 0.01

0.05 0.02 0.02 0.01 0.01 0.083

0.11 0.16 0.20 0.19 0.14 0.012

0.012 0.012 0.012 0.014 0.019 <0.012

<0.012 <0.012 <0.012 <0.012 0.012 0.013

0.014 0.016 0.014 0.025 0.033 0.130

0.198 0.220 0.258 0.251 0.214

### - 79 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330strawberry Glisolles, NFrance, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 7 14 <0.01

0.14 0.08 0.07 0.02 0.01 <0.012

0.086 0.078 0.11 0.12 0.060 <0.012

<0.012 <0.012 0.012 0.012 0.013 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

0.008 0.008 0.008 0.009 0.012 0.054

0.258 0.19 0.212 0.173 0.107 Field trials – Southern Europe strawberry San Martino,

Italy, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 7 14 <0.01

0.04 0.02 0.02 0.01 <0.01 <0.012

0.020 0.050 0.080 0.075 0.029 <0.012

<0.012 0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 0.012 <0.012 <0.008

<0.008 0.008 0.012 0.034 0.020 0.054

0.092 0.102 0.136 0.143 0.083 strawberry Imola, Italy,

2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 7 14 <0.01

0.05 0.02 0.01 <0.01 0.01 0.037

0.070 0.080 0.11 0.066 0.042 0.012

0.015 0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

0.008 <0.008 0.008 0.008 0.014 0.079

0.155 0.132 0.152 0.108 0.09 strawberry Sant Cebrià

de Vallalta, Spain, 2004 fruit

fruit fruit fruit fruit 0*

0 1 3 7 0.01

0.03 0.03 0.02 0.01 0.021

0.060 0.089 0.090 0.069 0.012

0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 0.008

0.008 0.008 0.008 0.009 0.063

0.122 0.151 0.143 0.114strawberry Courzieu, SFrance, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 7 15 0.01

0.10 0.06 0.02 0.01 0.02 0.052

0.058 0.049 0.061 0.019 0.012 0.012

0.015 0.015 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.011

0.011 0.012 0.008 0.008 0.008 0.097

0.197 0.144 0.113 0.061 0.054



### For the calculation of the MRL proposal, both of th e prescribed methods I and II have been used spirotetramat in strawberries (based on data obtain ed from trials from Northern and Southern Europe an d glasshouse):

MRL-calculation based on data obtained from the Nor thern Region: Individual data points for strawberry are: 0.162 mg/kg, 0.182 mg/kg, 0.212 mg/kg, 0.258 mg/kg Mean residue: 0.204 mg/kg; standard deviation: 0.04 2 mg/kg STMR: 0.197 mg/kg Highest residue: 0.258 mg/kg Method I: R max 

### = 0.418 mg/kg Method II: R ber 

### = 0.493 mg/kg Based on the data available for strawberry in North ern Europe, a MRL of 0.5 mg/kg can be proposed.

MRL-calculation based on data obtained from the Sou thern Region: Individual data points for strawberry are: 0.113 mg/kg, 0.143 mg/kg, 0.143 mg/kg, 0.152 mg/kg Mean residue: 0.138 mg/kg; standard deviation: 0.01 7 mg/kg STMR: 0.143 mg/kg Highest residue: 0.152 mg/kg Method I: R max 

### = 0.225 mg/kg

### - 80 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Method II: R ber 

### = 0.300 mg/kg Based on the data available for strawberry in South ern Europe, a MRL of 0.5 mg/kg can be proposed.

MRL-calculation based on data obtained from the gre enhouse trials: Individual data points for strawberry are: 0.205 mg/kg, 0.234 mg/kg, 0.244 mg/kg, 0.282 mg/kg, 0.282 mg/kg, 0.292 mg/kg, 0.303 mg/kg, 0.328 mg/kg Mean residue: 0.271 mg/kg; standard deviation: 0.04 0 STMR: 0.282 mg/kg Highest residue: 0.328 mg/kg Method I: R max 

### = 0.500 mg/kg Method II: R ber 

### = 0.601 mg/kg Based on the data available for strawberry in green house, a MRL of 1 mg/kg can be proposed.

Conclusion: In 2004, altogether 16 residue trials (field and gl asshouse) in Northern and Southern Europe were carr ied out. All trials were carried out according the inte nded use parameters and were performed as residue d ecline studies. The critical trials with highest residues levels were represented by the trials on protected crops. Outdoor studies showed lower residue levels which w ere 0.162 and 0.258 mg/kg in the four trials of the North and ranged between 0.113 and 0.152 mg/kg in t he Southern European trials. Therefore the 8 the greenhouse trials from Europe were taken for MRL ca lculation. Based on these trials a MRL of 1 mg/kg c an be proposed. Comments (RMS): All residue trials were performed only in one seaso n. But as the the highest residues were determined in the glasshouse trials the weather conditions in differe nt saisons should not influence the outcome of the residue trials.

B.7.6.6 Bulb vegetable

B.7.6.6.1 Onion

Spirotetramat is applied for control Thrips tabacch i in onion. The critical European GAP for the use i n northern (S-EU) and southern Europe (S-EU) is summa rized in Table B.7.6.6.1-1 Table B.7.6.6.1-1: GAP for residue situation in on ion

North or South of EU Indoor or

outdoor Number of

applications Mode of

application Growth stage at

last application Application rate expressed

under the relevant unit PHI (d) EU-N F 4 Spray BBCH 82 0.072 g a.s./ha 7



### Reference: Determination of the residues of BYI08330 in/on oni on after spraying of BYI08330 (100 OD) in the field in Germany and North ern France Author(s), year: Cavaille C.; 2005 Report/Doc. number: RA-2131/04, including trials no . R 2004 0854/4, R 2004 0855/2, R 2004 0856/0, R 2004 0857/9 M-259115-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

### - 81 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Reference: Determination of the residues of BYI08330 in/on oni on after spraying of BYI08330 (150 OD) in the field in United Kingdom, N orthern France and Germany Author(s), year: Ballesteros C.; Gateaud L.; 2006 Report/Doc. number: RA-2040/05, including trials no . R 2005 0212/5, R 2005 0214/1, R 2005 0216/8, R 2005 0217/6 M-269474-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the residues of BYI08330 in/on oni on after spraying of BYI08330 (100 OD) in the field in Southern France, Greece, Italy and Spain Author(s), year: Cavaille C.; 2005 Report/Doc. number: RA-2132/04, including trials no . R 2004 0858/7, R 2004 0859/5, R 2004 0860/9, R 2004 0861/7 M-259663-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the residues of BYI08330 in/on oni on after spraying of BYI08330 (150 OD) in the field in Italy, Spain and Southern France Author(s), year: Ballesteros C.; Gateaud L.; 2006 Report/Doc. number: RA-2041/05, including trials no . R 2005 0225/7, R 2005 0226/5, R 2005 0227/3, R 2005 0228/1 M-269869-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Experimental design: During 2004 and 2005, 8 residue trials for each Eur opean region were conducted. All studies were carri ed out using oil based dispersion concentrates contain ing 150 g/L and 100 g/L of spirotetramat respective ly. The product was used four times, using an applicati on rate of 0.072 kg a.s./ha. All trials were perfor med according to the critical European GAP. An overview on the supervised residue trials is giv en in Table B.7.6.6.1-2. Table B.7.6.6.1-2: Overview on supervised residue trials with BYI08330 on onion

Study no. Region Formulation No. of

trials Year Use rate

(g as/ha) Water

volume (L/ha) No of

appl. Spray

interval (days) PHI

days

RA-2131/04 N-EU OD 100 4 2004 72 400-600 4 7 7-21 RA-2040/05 N-EU OD150 4 2005 72 300/400 4 6-8 7-21 RA-2132/04 S-EU OD 100 4 2004 72 400-600 4 6-8 7-21 RA-2041/05 S-EU OD150 4 2005 72-78 500-646 4 6-9 7-21

### - 82 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

The last application was carried out at BBCH growth stage 47-48. Specimens of onion pulps were taken before the last treatment, 0, 3, 7, 14 and 21 days after the last application. All samples were stored deep frozen within 24 hours after sampling. The time intervals between date of deep-freezing and the last extraction ranged from 3 44 to 479 days for the trials carried out in 2004 a nd 84- 225 days for the residue trials from 2005. Analytical method used in all studies: Residues of spirotetramat and its metabolites BYI 0 8330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and BYI 08330-enol-Glc in onion were determ ined by HPLC-ESI-MS/MS according to method

00857. The limit of quantification (LOQ, defined as the lo west validated fortification level) was 0.01 mg/kg for spirotetramat, 0.012 mg/kg for its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and 0.008 mg/kg for BYI 08330-enol-Glc in/o n onion, all metabolites calculated as spirotetrama t equivalent. The mean procedural recoveries at the fortification levels of 0.01 to 1.0 mg/kg for spirotetramat and its four metabolites ranged between 78 and 100%. Findings: A detailed summary of the residue results is given in Appendix I i. The total residue of spirotetramat in onion bulbs f rom 8 field trials in northern Europe ranged betwee n <0.054 to 0.202 mg/kg. From the 8 field trials carried out in southern Europe, the total residues of <0.054 - 0.172 mg/kg were detected. The residue data used fo r the evaluation are marked in bold. There was no difference of residues in onion bulbs grown in nort hern or southern Europe. Major component of the total residue of BYI08330 in onion was BYI08330-enol. Table B.7.6.6.1-3: Overview of European residue da ta for spirotetramat and its metabolites in onion used 4 times with application rates of 0.076 kg a.s ./ha (residues are calculated as spirotetramat equivalent):

crop / formulatio

n Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 Field trials – Northern Europe Onion / 100 OD Langenfeld,

Germany, 2004 bulb

bulb bulb bulb 0

7 14 21 0.04

<0.01 <0.01 <0.01 0.16

0.16 0.051 0.060 <0.012

<0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 0.232

0.202 0.093 0.102 Onion / 100 OD Champien,

France, 2004 bulb

bulb bulb bulb 0

7 14 21 0.03

<0.01 <0.01 <0.01 0.061

0.055 0.045 0.052 <0.012

<0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 0.123

0.097 0.087 0.094 Onion / 100 OD Brüggen,

Germany, 2004 bulb

bulb bulb bulb bulb bulb 0

0 4 7 14 21 0.01

0.04 0.02 <0.01 <0.01 <0.01 0.061

0.063 0.066 0.055 0.066 0.067 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.103

0.135 0.118 0.097 0.108 0.109

Onion / 100 OD Epone,

France, 2004 bulb

bulb bulb bulb bulb bulb 0

0 3 7 14 21 <0.01

0.01 <0.01 <0.01 <0.01 <0.01 0.047

0.052 0.052 0.071 0.058 0.052 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.089

0.094 0.094 0.113 0.100 0.094 Onion / 150 OD thetford,

UK, 2005 bulb

bulb 0

8 0.01

<0.01 0.11

0.12 <0.012

<0.012 <0.012

<0.012 <0.008

<0.008 0.152

0.162

Onion / 150 OD Champien,

France, 2005 bulb

bulb 0

7 0.02

0.01 <0.012

<0.012 <0.012

<0.012 <0.012

<0.012 <0.008

<0.008 0.064

<0.054

### - 83 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / formulatio

n Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330

Onion / 150 OD LangenfeldRS-EUrath, Germany, 2005 bulb

bulb bulb bulb bulb bulb 0

0 3 7 14 21 <0.01

0.01 <0.01 <0.01 <0.01 <0.01 0.042

0.043 0.042 0.042 0.041 0.038 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.084

0.085 0.084 0.084 0.083 0.080 Onion / 150 OD Bornheim,

Germany, 2005 bulb

bulb bulb bulb bulb bulb 0

0 3 7 15 21 <0.01

0.04 0.01 <0.01 <0.01 <0.01 0.020

0.038 0.040 0.050 0.040 0.031 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.062

0.110 0.082 0.092 0.082 0.073 Field trials – Southern Europe

Onion / 100 OD Chazay

d'Azergues, France, 2004 bulb

bulb bulb bulb 0

7 14 21 <0.01

<0.01 <0.01 <0.01 0.040

0.021 0.024 0.022 <0.012

<0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 0.082

0.063 0.066 0.064 Onion / 100 OD Thiva,

Greece, 2004 bulb

bulb bulb bulb 0

7 14 21 <0.01

<0.01 <0.01 <0.01 0.064

0.081 0.061 0.055 <0.012

<0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 0.106

0.123 0.103 0.097 Onion / 100 OD Bologna,

Italy, 2004 bulb

bulb bulb bulb bulb bulb 0

0 3 7 14 21 0.02

0.02 <0.01 <0.01 <0.01 <0.01 0.042

0.038 0.050 0.052 0.052 0.056 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.094

0.090 0.092 0.094 0.094 0.098 Onion / 100 OD Alginet,

Spain, 2004 bulb

bulb bulb bulb bulb bulb 0

0 3 7 14 21 <0.01

0.01 <0.01 <0.01 <0.01 <0.01 0.090

0.083 0.11 0.13 0.12 0.11 <0.012

<0.012 <0.012 0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.132

0.125 0.152 0.172 0.162 0.152 Onion / 150 OD Settepolesini,

Italy, 2005 bulb

bulb 0

7 <0.01

<0.01 0.030

0.034 <0.012

<0.012 <0.012

<0.012 <0.008

<0.008 0.072

0.076

Onion / 150 OD Malgrat de

Mar, Spain, 2005 bulb

bulb 0

7 0.02

0.02 0.032

0.037 <0.012

0.017 <0.012

<0.012 <0.008

<0.008 0.084

0.094

Onion / 150 OD Saint Jory ,

France, 2005 bulb

bulb bulb bulb bulb bulb 0

0 3 7 14 21 <0.01

0.01 0.01 <0.01 <0.01 <0.01 0.037

0.051 0.14 0.10 0.050 0.034 <0.012

0.015 <0.012 0.013 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.079

0.096 0.182 0.143 0.092 0.076 Onion / 150 OD Alginet,

Spain, 2005 bulb

bulb bulb bulb bulb bulb 0

0 3 7 14 21 <0.01

<0.01 <0.01 <0.01 <0.01 <0.01 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.054

<0.054 <0.054 <0.054 <0.054 <0.054



### For the calculation of the MRL proposal, both of th e prescribed methods I and II have been used spirotetramat in onion (based on data obtained from trials from Northern and Southern Europe):

### - 84 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

MRL-calculation based on data obtained from the Nor thern Region: Individual data points for onion are: <0.054, 0.084, 0.092, 0.097, 0.109, 0.113, 0.162, 0 .202 mg/kg Mean residue: 0.114 mg/kg; standard deviation: 0.04 7 mg/kg STMR: 0.103 mg/kg Highest residue: 0.202 mg/kg Method I: R max 

### = 0.263 mg/kg Method II: R ber 

### = 0.300 mg/kg Based on the data available for onion in Northern E urope, a MRL of 0.3 mg/kg can be proposed.

MRL-calculation based on data obtained from the Sou thern Region: Individual data points for onion are: <0.054, 0.066, 0.076, 0.094, 0.098, 0.123, 0.143, 0 .172 mg/kg Mean residue: 0.103 mg/kg; standard deviation: 0.04 0 mg/kg STMR: 0.096 mg/kg Highest residue: 0.172 mg/kg Method I: R max 

### = 0.232 mg/kg Method II: R ber 

### = 0.276 mg/kg Based on the data available for onion in Southern E urope, a MRL of 0.3 mg/kg can be proposed.

Conclusion: In 2004 and 2005, altogether 16 residue trials in N orthern and Southern Europe were carried out. Al tr ials were carried out according the intended use paramet ers. All residue trials were performed as residue d ecline studies. There was no difference of residues in oni on bulbs grown in northern or southern Europe. Base d on the submitted supervised residue trials a MRL of 0.3 mg/kg can be proposed. Comments (RMS): No comments.

B.7.6.7 Fruiting vegetables

B.7.6.7.1 Tomato

Spirotetramat is applied the use in tomatoes agains t whiteflies, aphids, and mites. The critical Europ ean GAPs in the greenhouse and in the field use in sout hern Europe (S-EU) are summarized in Table B.7.6.7. 1-

1. Table B.7.6.7.1-1: GAP for residue situation in to matoes

North or South of EU Indoor or

outdoor Number of

applications Mode of

application Growth stage at

last application Application rate expressed

under the relevant unit PHI (d) EU-S F 4 Spray BBCH 87 0.072 g a.s./ha 3 EU-N/S G 4 Spray BBCH 87 0.072 kg a.s./ha and m leafy surface, max. 0.144 kg a.s./ha 3

### - 85 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Reference: Determination of the Residues of BYI08330 in/on Che rry Tomato After Spraying of BYI08330 (100 OD) in the Greenhouse in Italy and Spain Author(s), year: Freitag T.; Helfrich P.; 2006 Report/Doc. number: RA-2139/04, including trials no . R 2004 0823/4, R 2004 0824/2, R 2004 0825/0, R 2004 0826/9 M-264462-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the Residues of BYI08330 in/on Tom ato after Spraying of BYI08330 (100 OD) in the Greenhouse in Greece, Spai n and Italy Author(s), year: Freitag T.; Helfrich P.; 2005 Report/Doc. number: RA-2140/04, including trials no . R 2004 0827/7, R 2004 0828/5, R 2004 0829/3, R 2004 0830/7 M-263523-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the Residues of BYI08330 in/on Tom ato after Spraying of BYI08330 (100 OD) in the Field in Spain, Portugal, Greece and Italy Author(s), year: Freitag T.; Helfrich P.; 2006 Report/Doc. number: RA-2130/04, including trials no . R 2004 0849/8, R 2004 0850/1, R 2004 0852/8, R 2004 0853/6 M-263566-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Experimental design: The magnitude of residues of spirotetramat and its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-mono-hydroxy and BYI 08330-enol-Glc in tomato es harvested following four applications with the formulation BYI 08330 100 OD in Southern Europe (4 trials: Italy, Greece, Spain and Portugal) and tria ls in greenhouses (8 trials) was determined. All trials w ere carried out in 2004. The used formulation was the oil based dispersion c oncentrates containing 100 g/L spirotetramat. For t he greenhouse applications, the product was used four times at application rates of 0.072 kg a.s./ha and meter leafy surface and a water volume of 750 – 1000 L pe r ha and meter leafy surface (1.45 – 2.2 m), this i s corresponding to 0.104 – 0.166 kg a.s./ha. An overv iew on the supervised residue trials conducted with BYI 08330 100 OD formulation is given in Table B.7.6.5. 2-2 Table B.7.6.7.1-2: Overview on European residue tr ials with BYI08330 in tomatoes

Location Formulation No. of trials Year Use rate

(g as/ha) Water volume No of appl. Spray interval

(days)

Greenhouse OD 100 4 2004 108-166* 1600-1760 4 6-7

### - 86 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Location Formulation No. of trials Year Use rate

(g as/ha) Water volume No of appl. Spray interval

(days)

Greenhouse OD 100 4 2004 108-144* 1125-1600 4 6-7 Field S-EU OD 100 4 2004 72 750 4 6-9 * corresponding to 72 g a.s./ha per meter leafy sur face



### The last applications were carried out at growth st age between BBCH 72 and BBCH 87. Samples were taken before the last application, 0, 1, 3, 4-5 and 7-8 d ays after the last application. All samples were stored deep frozen within 24 hours after sampling. The time intervals between date of deep-freezing and the last extraction ranged from 1 22 to 265 days. Analytical method used in all studies: Residues of spirotetramat and its metabolites BYI 0 8330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and BYI 08330-enol-Glc were determined by H PLC-ESI-MS/MS according to method 00857. The limit of quantification (LOQ, defined as the lowest validated fortificatio n level) was 0.01 mg/kg for spirotetramat, 0.012 mg/kg for its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and 0.008 mg/kg for BYI 08330-enol-Glc in/o n tomatoes (all metabolites calculated as spirotetr amat equivalent). The mean procedural recoveries at the fortification levels of 0.01 to 2.0 mg/kg f or spirotetramat and its four metabolites ranged between 78 and 101 % and RSD < 2 0%; these results indicate that the methods used were suitable for this analysis. Findings: A detailed summary of the residue results is given in Appendix I j. The total residue of spirotetramat in tomatoes grow n in the greenhouse (8 trials) according to the Eur opean GAP ranged between 0.215 and 0.736 mg/kg. In tomato es from 4 field trials in southern Europe a total residue of 0.120 to 0.209 mg/kg could be determined . The results indicated that the residue level in t omatoes grown in greenhouse is higher than in the field tri als. Therefore, for estimation of the dietary risk and for MRL setting, the residue results from the 8 greenhouse residue trials were taken in consideration. General ly residue data of day 3 after the last application we re evaluated according to the PHI of the critical E uropean GAP. If the total residue of spirotetramat at longe r intervals exceeded the residue of day 3, the high er value was evaluated to cover the worst case residue. An o verview of the residue data is reported in the tabl e below. The residue data used for the evaluation are marked in bold. The total residues of spirotetramat in tomato fruit s are mainly composed of the parent compound and th e enol metabolite. BYI08330-ketohydroxy and -enol-glu coside were minor metabolites. BYI08330- monohydroxy was not found. Table B.7.6.7.1-3: Overview of European residue dat a for spirotetramat and its metabolites in tomatoes used 4 times with application rates of 0.0 76 kg a.s./ha (residues are calculated as spirotetramat equivalent); formulation: BYI 08330 1 00 OD

crop Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330

Greenhouse trials cherry tomato, Giovinazzo,

Italy, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 4 8 0.12

0.25 0.11 0.09 0.11 0.05 0.20

0.21 0.19 0.18 0.17 0.16 0.065

0.056 0.040 0.039 0.050 0.032 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.080

0.084 0.082 0.096 0.10 0.11 0.477

0.612 0.434 0.417 0.442 0.364 cherry tomato Molfetta

(Bari), Italy, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 4 8 0.12

0.19 0.10 0.04 0.16 0.14 0.16

0.14 0.17 0.17 0.16 0.15 0.019

0.019 0.014 0.012 0.022 0.020 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.065

0.059 0.062 0.061 0.082 0.094 0.376

0.420 0.358 0.295 0.436 0.416

### - 87 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 cherry tomato Jayena

Granada, Spain, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 0.18

0.39 0.24 0.22 0.25 0.25 0.22

0.27 0.23 0.25 0.24 0.21 0.013

0.017 0.016 0.022 0.021 0.024 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.15

0.17 0.15 0.17 0.18 0.24 0.575

0.859 0.648 0.674 0.703 0.736 cherry tomato Fornes

Granada, Spain, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 0.23

0.27 0.22 0.25 0.16 0.16 0.22

0.21 0.20 0.23 0.23 0.21 0.044

0.037 0.033 0.045 0.036 0.034 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.12

0.11 0.12 0.14 0.14 0.19 0.626

0.639 0.585 0.677 0.578 0.606 Tomato Vasilica,

Greece, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 8 0.04

0.05 0.04 0.06 0.03 0.03 0.11

0.11 0.19 0.39 0.23 0.18 0.012

0.012 0.012 0.021 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.026

0.019 0.021 0.031 0.028 0.030 0.200

0.203 0.275 0.514 0.312 0.264 Tomato Palacios

Sevilla, Spain, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 6 7 0.09

0.10 0.10 0.09 0.04 0.09 0.077

0.078 0.093 0.10 0.081 0.099 0.012

0.012 0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.039

0.040 0.042 0.043 0.048 0.078 0.230

0.242 0.259 0.257 0.193 0.291 Tomato Viladecans,

Spain, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 4 7 0.11

0.13 0.14 0.15 0.15 0.14 0.093

0.073 0.075 0.11 0.079 0.11 0.012

0.012 0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.034

0.034 0.034 0.052 0.039 0.062 0.261

0.261 0.273 0.336 0.292 0.336 Tomato Vittoria (RG),

Italy, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 0.03

0.06 0.06 0.07 0.03 0.03 0.070

0.073 0.079 0.093 0.084 0.095 0.012

0.012 0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.020

0.021 0.021 0.028 0.035 0.040 0.144

0.178 0.184 0.215 0.173 0.189 Field trials – Southern Europe Tomato L'Hospitalet

de Llobregat, Spain, 2004 fruit

fruit fruit fruit fruit 0

3 6 7 13 0.04

0.02 0.04 0.03 0.01 0.045

0.058 0.088 0.092 0.075 0.012

<0.012 0.012 0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 0.018

0.023 0.036 0.041 0.041 0.127

0.125 0.188 0.187 0.150 Tomato Vale de

Cavalos, Portugal, 2004 fruit

fruit fruit fruit fruit 0

3 5 7 14 0.06

0.04 0.03 0.02 0.01 0.056

0.061 0.057 0.059 0.048 0.012

0.012 0.012 0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 0.018

0.019 0.026 0.026 0.030 0.158

0.144 0.137 0.129 0.112 Tomato Petra,

Greece, 2004 fruit

fruit fruit fruit fruit fruit fruit 0*

0 1 3 5 7 14 0.01

0.05 0.04 0.02 0.02 0.02 0.01 0.035

0.057 0.057 0.038 0.045 0.041 0.034 0.012

0.012 0.012 0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.017

0.024 0.024 0.023 0.031 0.026 0.038 0.086

0.155 0.145 0.105 0.120 0.111 0.106

### - 88 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330

Tomato Zapponeta

(Fg), Italy, 2004 fruit

fruit fruit fruit fruit fruit fruit 0*

0 1 3 5 7 14 0.01

0.03 0.03 0.03 0.03 0.04 0.04 0.13

0.13 0.12 0.13 0.11 0.065 0.074 0.012

0.012 0.012 0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.012

0.013 0.015 0.025 0.023 0.022 0.042 0.176

0.197 0.189 0.209 0.187 0.151 0.180



### For the calculation of the MRL proposal, both of th e prescribed methods I and II have been used spirotetramat in tomatoes (based on data obtained f rom trials from Southern Europe and greenhouse):

MRL-calculation based on data obtained from the Sou thern Region (field): Individual data points for tomato are: 0.12, 0.144, 0.188, 0.209 mg/kg Mean residue: 0.165 mg/kg; standard deviation: 0.04 1 mg/kg STMR: 0.166 mg/kg Highest residue: 0.209 mg/kg Method I: R max 

### = 0.374 mg/kg Method II: R ber 

### = 0.408 mg/kg Based on the data available for tomato in Southern Europe, a MRL of 0.5 mg/kg can be proposed.

MRL-calculation based on data obtained from the gre enhouse trials: Individual data points for tomato are: 0.215, 0.291, 0.336, 0.436, 0.442, 0.514, 0.677, 0. 736 mg/kg Mean residue: 0.456 mg/kg; standard deviation: 0.18 2 STMR: 0.439 mg/kg Highest residue: 0.736 mg/kg Method I: R max 

### = 1.035 mg/kg Method II: R ber 

### = 1.273 mg/kg Based on the data available for tomato in greenhous e, a MRL of 2 mg/kg can be proposed.

Conclusion: In 2004, altogether 12 residue trials (4 field tria ls in southern Europe and 8 trials in glasshouses) were carried out. Al trials were carried out according t he intended use parameters and performed as residue decline studies. The critical trials with highest r esidues levels were represented by the trials on pr otected crops. The results of the four field trials carried out in southern Europe resulted in lower residue l evels (0.120 – 0.209 mg/kg total residues of spirotetramat). The refore the 8 European greenhouse trials were taken for MRL proposal. Based on these trials a MRL of 2 mg/k g can be proposed. Comments (RMS): All residue trials were performed only in one seaso n. But as the the highest residues were determined in the glasshouse trials the weather conditions in differe nt saisons should not influence the outcome of the residue trials and the consumer risk asessment.

B.7.6.7.2 Pepper

Spirotetramat is applied for the use in peppers aga inst aphids, scales and mites. The critical Europea n GAPs in the greenhouse and in the field in southern Euro pe (S-EU) are summarized in Table B.7.6.7.2-1.

### - 89 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.6.7.2-1: GAP for residue situation in pe ppers North or South of EU Indoor or

outdoor Number of

applications Mode of

application Growth stage at

last application Application rate expressed

under the relevant unit PHI (d) EU-S F 4 Spray BBCH 87 0.072 g a.s./ha 3 EU-N/S G 4 Spray BBCH 87 0.072 kg a.s./ha and m leafy surface, max. 0.144 kg a.s./ha 3



### Reference: Determination of the Residues of BYI08330 in/on Pep per after Spraying of BYI08330 (100 OD) in the Greenhouse in the Netherla nds, Germany, southern France, Portugal, Italy and Spain Author(s), year: Schöning R.; Wolters A.; 2005 Report/Doc. number: RA-2026/04, including trials no . R 2004 0113/2, R 2004 0114/0, R 2004 0115/9, R 2004 0116/7, R 2004 0117/5, R 2004 0118/3, R 2004 0 119/1, R 2004 0120/5 M-259820-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the Residues of BYI08330 in/on Pep per after Spraying of BYI08330 (100 OD) in the Field in Spain, southern F rance, Italy and Portugal Author(s), year: Schöning R.; Wolters A.; 2005 Report/Doc. number: RA-2027/04, including trials no . R 2004 0121/3, R 2004 0122/1, R 2004 0124/8, R 2004 0125/6 M-260011-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the Residues of BYI08330 in/on Pep per after spraying of BYI08330 (240 SC) in the Greenhouse in Southern Fra nce, Germany, Italy and Portugal Author(s), year: Schöning R.; Helfrich P.; 2006 Report/Doc. number: RA-2134/04, including trials no . R 2004 0791/2, R 2004 0792/0, R 2004 0793/9, R 2004 0794/7 M-263426-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

### - 90 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Reference: Determination of the Residues of BYI08330 in/on Pep per after Spraying of BYI08330 (150 OD) in the Field in Italy and Portuga l Author(s), year: Schöning R.; Wolters A.; 2006 Report/Doc. number: RA-2039/05, including trials no . R 2005 0200/1, R 2005 0202/8 M-266615-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the Residues of BYI08330 in/on Pep per after Spraying of BYI08330 (048 SC) in the Field in Italy and Portuga l Author(s), year: Schöning R.; Wolters A.; 2006 Report/Doc. number: RA-2046/05, including trials no . R 2005 0707/0, R 2005 0708/ M-266682-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Experimental design: For southern Europe, 8 residue field trials were co nducted on pepper. As test substance the oil based dispersion concentrates 100 OD and 150 OD and a sus pensions concentrate 048 OD were used. 12 residue trials were carried out under greenhouse conditions using 100 OD and 240 SC formulations as test substances. In the greenhouse trials the use rate o f spirotetramat was adapted to the height of the le afy surface of the pepper plants. The plant height at t he last application was between 0.7 and 1.9 m. Henc e, the application rate per ha ranged between 0.068 and 0. 137 kg as/ha and a water volume of 750 – 1000 l/ha and meter leafy surface. An overview on the use pattern of the supervised re sidue trials conducted with different formulations of BYI08330 is given in Table B.7.6.7.2-2. Table B.7.6.7.2-2: Overview on European residue tr ials with BYI08330 in peppers

Location Formulation No. of trials Year Use rate

(g as/ha) Water volume No of appl. Spray interval

(days)

Greenhouse 100 OD 8 2004 43.2-137* 450-1900 L/ha 4 6-8 Greenhouse 240 SC** 4 2004 43.2-108* 450-1125 L/ha 4 6-7 Field EU-S OD 100 4 2004 72 600-1000 L/ha 4 6-7 Field EU-S OD 150 2 2005 72 500, 800 L/ha 4 7 Field EU-S OD 150 2 2005 72 500, 800 L/ha 4 7 * corresponding to 72 g a.s./ha per meter leafy sur face ** additive RME 500EW, 0.2% was added to the spray liquid at each application



### The last application was carried out at BBCH growth stage 68-85. Samples were taken before the last application, 0, 1, 3, 4-6 and 7 days after the last application. All samples were stored deep frozen within 24 hours after sampling. The time intervals between date of deep-freezing and the last extraction ranged from 7 0 to 205 days. Analytical method used in all studies: Residues of spirotetramat and its metabolites BYI 0 8330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and BYI 08330-enol-Glc were determined by H PLC-ESI-MS/MS according to method 00857.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

The limit of quantification (LOQ, defined as the lowest validated fortificatio n level) was 0.01 mg/kg for spirotetramat, 0.012 mg/kg for its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and 0.008 mg/kg for BYI 08330-enol-Glc in/o n pepper (all metabolites calculated as spirotetram at equivalent). The mean procedural recoveries at the fortification levels of 0.01 to 1.0 mg/kg f or spirotetramat and its four metabolites ranged between 84 and 106 % and RSD < 2 0%; these results indicate that the methods used were suitable for this analysis. Findings: A detailed summary of the residue results is given in Appendix I k. The total residue of spirotetramat in peppers grown in the greenhouse (12 trials) according to the Eur opean GAP ranged between 0.268 and 0.581 mg/kg. In pepper , from 8 field trials in southern Europe a total re sidue of 0.113 to 0.817 mg/kg could be determined. Genera lly residue data of day 3 after the last applicatio n were evaluated according to the PHI of the critical Euro pean GAP. If the total residue of spirotetramat at longer intervals exceeded the residue of day 3, the higher value was evaluated to cover the worst case residu e. An overview of the residue data is reported in the tab le below. The residue data used for the evaluation are marked in bold. To determine the influence of different formulation s (SC and OD) on the residue behaviour of BYI08330 residues in pepper grown in the greenhouse and trea ted with BYI08330 OD 100 or SC 240 + RME were compared. Moreover, residues from field trials cond ucted with the SC 048 formulation were compared to residues in pepper treated with the OD 100 and 150 formulations. The results are corresponding with th e total residue in pepper after application of the OD formulations. Main component of the total residue of spirotetrama t in pepper is BYI08330-enol. The parent compound, BYI08330-ketohydroxy and BYI08330-enol-glucoside ar e minor components. BYI08330-monohydroxy was not detected in pepper fruit or in traces, only.

Table B.7.6.7.2-3: Overview of European residue dat a for spirotetramat and its metabolites in pepper used 4 times with application rates of 0.076 kg a.s ./ha (residues are calculated as spirotetramat equivalent):

crop / formulatio

n Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330

Greenhouse trials Pepper, sweet 100 OD Heerhugowaard, Netherlands, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 0.05

0.10 0.07 0.08 0.05 0.04 0.35

0.38 0.40 0.41 0.39 0.46 0.021

0.021 0.024 0.024 0.022 0.027 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.016

0.017 0.018 0.021 0.023 0.026 0.449

0.530 0.524 0.547 0.497 0.565 Pepper, sweet 100 OD Leichlingen,

Germany, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 4 7 0.06

0.11 0.09 0.07 0.07 0.04 0.39

0.36 0.39 0.38 0.40 0.46 0.021

0.021 0.021 0.022 0.025 0.021 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.054

0.044 0.053 0.048 0.053 0.048 0.537

0.547 0.566 0.532 0.560 0.581 Pepper, sweet 100 OD Graveson, SFrance, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 0.03

0.07 0.06 0.05 0.04 0.04 0.25

0.29 0.28 0.31 0.32 0.29 0.024

0.041 0.028 0.027 0.029 0.025 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.019

0.022 0.020 0.022 0.025 0.025 0.335

0.435 0.400 0.421 0.426 0.392

### - 92 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / formulatio

n Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 Pepper, sweet 100 OD Póvoa da

Isenta, Portugal, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 6 7 0.03

0.06 0.03 0.03 0.04 0.02 0.29

0.28 0.25 0.25 0.26 0.25 0.027

0.030 0.026 0.019 0.023 0.019 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.013

0.013 0.014 0.014 0.016 0.018 0.372

0.395 0.332 0.325 0.351 0.319 Pepper, sweet 100 OD Molfetta

(Bari), Italy, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 0.08

0.14 0.08 0.12 0.08 0.13 0.23

0.25 0.25 0.31 0.31 0.34 0.015

0.017 0.015 0.021 0.019 0.025 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.019

0.023 0.020 0.027 0.030 0.039 0.356

0.442 0.377 0.490 0.451 0.546 Pepper, sweet 100 OD Leichlingen,

Germany, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 4 7 0.05

0.11 0.08 0.07 0.05 0.05 0.32

0.30 0.33 0.26 0.30 0.35 0.018

0.016 0.019 0.015 0.019 0.018 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.052

0.036 0.040 0.039 0.046 0.050 0.452

0.474 0.481 0.396 0.427 0.480 Pepper, sweet 100 OD Pernes les

Fontaines, SFrance, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 0.02

0.03 0.03 0.03 0.01 0.02 0.17

0.18 0.19 0.20 0.20 0.18 0.014

0.017 0.017 0.016 0.017 0.015 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.010

0.010 0.010 0.010 0.013 0.013 0.226

0.249 0.259 0.268 0.252 0.240 Pepper, sweet 100 OD Mataró,

Spain, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 4 7 0.03

0.05 0.06 0.03 0.03 0.03 0.37

0.38 0.42 0.38 0.42 0.43 0.018

0.019 0.020 0.019 0.020 0.020 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.052

0.034 0.029 0.036 0.027 0.044 0.482

0.495 0.541 0.477 0.509 0.536 Pepper, sweet 240 SC Graveson, SFrance, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 0.03

0.06 0.06 0.06 0.05 0.04 0.28

0.30 0.31 0.36 0.32 0.29 0.029

0.028 0.032 0.025 0.028 0.029 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.022

0.023 0.021 0.026 0.028 0.029 0.373

0.423 0.435 0.483 0.438 0.400 Pepper, sweet 240 SC Leichlingen,

Germany, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 4 7 0.09

0.18 0.13 0.12 0.12 0.12 0.21

0.23 0.28 0.26 0.27 0.37 0.013

0.015 0.016 0.016 0.017 0.021 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.026

0.027 0.033 0.038 0.031 0.051 0.351

0.464 0.471 0.446 0.450 0.574 Pepper, sweet 240 SC Molfetta

(Bari), Italy, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 0.08

0.16 0.12 0.10 0.06 0.12 0.10

0.11 0.11 0.13 0.13 0.15 0.012

0.012 0.012 0.012 0.012 0.013 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.008

0.008 0.009 0.009 0.010 0.016 0.212

0.302 0.263 0.263 0.224 0.311 Pepper, sweet 240 SC Póvoa da

Isenta, Portugal, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 6 7 0.04

0.09 0.05 0.04 0.02 0.03 0.20

0.20 0.21 0.21 0.18 0.19 0.013

0.023 0.015 0.014 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.010

0.012 0.011 0.013 0.013 0.017 0.275

0.337 0.298 0.289 0.237 0.260

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / formulatio

n Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 Field trials – Southern Europe Pepper, sweet 100 OD Alginet,

Spain, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 6 7 0.13

0.28 0.20 0.14 0.08 0.10 0.51

0.51 0.55 0.54 0.51 0.48 0.034

0.039 0.057 0.062 0.047 0.053 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.051

0.043 0.050 0.063 0.053 0.066 0.737

0.884 0.869 0.817 0.702 0.711 Pepper, sweet 100 OD Le Burgaud,

France, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 <0.01

0.01 0.01 0.01 <0.01 <0.01 0.19

0.19 0.15 0.21 0.18 0.21 0.012

0.012 0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.016

0.014 0.013 0.019 0.017 0.022 0.24

0.238 0.197 0.263 0.231 0.266 Pepper, sweet 100 OD Giovinazzo

(Bari), Italy, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 <0.01

0.01 0.01 0.01 <0.01 <0.01 0.11

0.12 0.13 0.13 0.16 0.12 0.012

0.012 0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.010

0.009 0.009 0.010 0.012 0.011 0.154

0.163 0.173 0.174 0.206 0.165 Pepper, sweet 100 OD Salvaterra,

Portugal, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 0.02

0.04 0.04 0.02 0.02 0.02 0.23

0.25 0.24 0.25 0.29 0.29 0.012

0.012 0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.015

0.014 0.013 0.015 0.018 0.019 0.289

0.328 0.317 0.309 0.352 0.353 Pepper, sweet 150 OD Canosa

(Bari), Italy, 2005 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 0.01

0.03 0.04 0.02 0.01 0.01 0.058

0.048 0.049 0.052 0.067 0.092 0.012

0.012 0.012 0.012 0.012 0.013 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.008

0.008 0.008 0.008 0.010 0.012 0.100

0.110 0.121 0.104 0.111 0.139 Pepper, sweet 150 OD CaniceiraVale de Cavalos, Portugal, 2005 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 0.01

0.03 0.01 0.01 0.01 0.01 0.13

0.15 0.13 0.12 0.13 0.098 0.012

0.012 0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.008

0.008 0.008 0.008 0.008 0.008 0.172

0.212 0.172 0.162 0.172 0.140 Pepper, sweet 048 SC Canosa di

Puglia (Bari), Italy, 2005 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 0.01

0.04 0.03 0.02 0.01 0.01 0.043

0.050 0.044 0.053 0.047 0.069 0.012

0.012 0.012 0.014 0.012 0.013 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.008

0.008 0.008 0.008 0.008 0.009 0.085

0.122 0.106 0.107 0.089 0.113 Pepper, sweet 048 SC Caniceira -

Vale de Cavalos, Portugal, 2005 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 0.01

0.04 0.02 0.02 0.02 0.01 0.089

0.11 0.096 0.12 0.11 0.11 0.012

0.012 0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.008

0.008 0.008 0.008 0.008 0.008 0.131

0.182 0.148 0.172 0.162 0.152



### For the calculation of the MRL proposal, both of th e prescribed methods I and II have been used spirotetramat in peppers (based on data obtained fr om trials from Southern Europe and greenhouse):

### - 94 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

MRL-calculation based on data obtained from the Sou thern Region (field): Individual data points for pepper are: 0.113, 0.139, 0.172, 0.172, 0.205, 0.266, 0.353, 0. 817 mg/kg Mean residue: 0.280 mg/kg; standard deviation: 0.23 0 mg/kg STMR: 0.189 mg/kg Highest residue: 0.817 mg/kg Method I: R max 

### = 1.013 mg/kg Method II: R ber 

### = 0.663 mg/kg Based on the data available for pepper in Southern Europe , a MRL of 2 mg/kg can be proposed.

MRL-calculation based on data obtained from the gre enhouse trials: Individual data points for pepper are: 0.268, 0.289, 0.311, 0.351, 0.426, 0.48, 0.483, 0.5 36, 0.546, 0.565, 0.574, 0.581 mg/kg Mean residue: 0.451 mg/kg; standard deviation: 0.18 2 STMR: 0.482 mg/kg Highest residue: 0.581 mg/kg Method I: R max 

### = 0.774 mg/kg Method II: R ber 

### = 1.121 mg/kg Based on the data available for pepper in greenhouse , a MRL of 2 mg/kg can be proposed. Conclusion: 20 trials were carried out in greenhouse all over E urope regions during 2004 and 2005 (8 field trials and 12 trials glasshouse trials). Spirotetramat is not int ended to be used as an outdoor crop in northern Eur ope, therefore supervised outdoor residue trials were ca rried out in Southern European regions only. There was no significant difference between the residues in p epper grown in southern Europe and in glasshouses. Based on the submitted supervised residue trials a MRL of 2 mg/kg can be proposed. Comments (RMS): No comments.

B.7.6.7.3 Cucumber

Spirotetramat is applied for the use in cucumber ag ainst aphids, whiteflies and mites. The critical Eu ropean GAPs for the greenhouse and field uses of BYI08330 in cucumber are summarised in Table B.7.6.7.3-1. Table B.7.6.7.3-1: GAP for residue situation in cu cumbers

North or South of EU Indoor or

outdoor Number of

applications Mode of

application Growth stage at

last application Application rate expressed

under the relevant unit PHI (d) EU-S F 4 Spray BBCH 87 0.072 g a.s./ha 3 EU-N/S G 4 Spray BBCH 87 0.072 kg a.s./ha and m leafy surface, max. 0.144 kg a.s./ ha 3



### Reference: Determination of the residues of BYI08330 in/on cuc umber after spraying of BYI08330 (100 OD) in the greenhouse in Germany, Ita ly, Spain and Greece Author(s), year: Cavaille C.; 2005 Report/Doc. number: RA-2030/04, including trials no . R 2004 0130/2, R 2004 0131/0, R 2004 0132/9, R 2004 0133/7, R 2004 0134/5, R 2004 0135/3, R 2004 0 136/1, R 2004 0138/8 M-259128-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

### - 95 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Reference: Determination of the residues of BYI08330 in/on cuc umber after spraying of BYI08330 (100 OD) in the field in Spain and Italy Author(s), year: Cavaille C.; 2005 Report/Doc. number: RA-2028/04, including trials no . R 2004 0126/4, R 2004 0128/0, R 2004 0129/9 M-259667-01-1 Guideline(s): GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the residues of BYI08330 in/on cuc umber after spraying of BYI08330 (150 OD) in the field in Spain and Italy Author(s), year: Ballesteros C.; 2005 Report/Doc. number: RA-2043/05, including trials no . R 2005 0239/7, R 2005 0240/0, R 2005 0241/9, R 2005 0715/1 M-268869-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Experimental design: For the magnitude of residues of spirotetramat and its metabolites BYI 08330-enol, BYI 08330-ketohydro xy, BYI 08330-mono-hydroxy and BYI 08330-enol-Glc in cu cumbers 7 trials in southern Europe and 8 trials under glasshouse conditions were performed. All tri als were carried out with oil based dispersion concentrates containing 100 and 150 g a.s./L respec tively. Spirotetramat was used four times in applic ation rates of 72 g a.s./ha and spray volumes between 600 and 1000 L/ha. For the greenhouse application, the product was used four times at application rates of 0.072 kg a.s./ha and meter leafy surface and a wat er volume of 750 L/ha and meter leafy surface (0.5 – 2 . m), this is corresponding to 0.036 – 0.144 kg a.s ./ha and a spray volume of 375 – 1500 L/ha. An overview on the supervised residue trials conducted with BYI 08330 OD formulations is given in Table B.7.6.7.3-2 Table B.7.6.7.3-2: Overview on European residue tr ials with spirotetramat in cucumbers

Location Formulation No. of trials Year Use rate

(g as/ha) Water volume No of appl. Spray interval

(days)

Greenhouse OD 100 8 2004 36-144* 375-1500 L/ha 4 5- 7 Field S-EU OD 100 3 2004 72 600-1000 L/ha 4 7 Field S-EU OD 150 4 2005 72 600-1000 L/ha 4 7-8 * corresponding to 72 g a.s./ha per meter leafy sur face



### The last applications were carried out at growth st age between BBCH 73 and BBCH 89. Samples were taken before the last application, 0, 1, 3, 5-6 and 7 day s after the last application. All samples were stored deep frozen within 24 hours after sampling. The time intervals between date of deep-freezing and the last extraction ranged from 1 99 to 445 days for the trials carried out in 2004 a nd 77- 142 days for the residue trials from 2005. Analytical method used in all studies: Residues of spirotetramat and its metabolites BYI 0 8330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and BYI 08330-enol-Glc were determined by H PLC-ESI-MS/MS according to method 00857. The limit of quantification (LOQ, defined as the lowest validated fortificatio n level) was 0.01 mg/kg for spirotetramat, 0.012 mg/kg for its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-mono-

### - 96 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

hydroxy and 0.008 mg/kg for BYI 08330-enol-Glc in/o n cucumbers (all metabolites calculated as spirotetramat equivalent). The mean procedural recoveries at the fortification levels of 0.01 to 1.0 mg/kg f or spirotetramat and its four metabolites ranged between 85 and 100 % and RSD < 2 0%; these results indicate that the methods used were suitable for this analysis. Findings: A detailed summary of the residue results is given in Appendix I l. 8 supervised residue trials with spirotetramat in c ucumber were performed in glasshouse in 2004 and altogether 7 trials were carried out in southern Eu rope in 2004 and 2005. The total residues of spirot etramat in cucumbers grown in the greenhouse ranged between <0.054 and 0.077 mg/kg In cucumbers from 7 field trials in southern Europe total residues of <0.054 to 0.119 mg/kg were determined: In cucumbers from o ne of the 7 field trials (R 2005 0715/1) the total residu e of spirotetramat was 0.119 mg/kg. In the study re port (No.: RA-2043/05) a deviation concerning this trial (Tria l No. R 2005 0715/1) was reported. Due to heavy wea ther conditions the crops from the primary performed tri al were damaged. The trial was restarted in October 2005. But the daily mean temperatures during the trial pr ocess were 5-16°C. Fruits were small (average weigh t 111-172 g) compared to cucumbers from the other tri als conducted from June until August 2005: R 2005 0239/7 (411-528 g), R 2005 0240/0 (227-318 g) and R 2005 0241/9 (236-270 g). Therefore, the higher residues in cucumber from trial R 2005 0715/1 can b e explained by lower temperatures slowing down metabolic processes and by the smaller size of the cucumber accompanied with a higher surface/volume ratio leading to higher residues expressed in mg/kg . This value was not excluded as an outlier, becaus e growing of cucumber in October/November is accordin g to agricultural practice in southern European countries although main growing season is summer. All trials were performed according the intended Eu ropean GAPs. An overview of the residue data is reported in the table below. The residue data used for the evaluation are marked in bold. The main component of the total residue was parent compound. In addition, traces of enol or ketohydrox y were found. BYI08330-monohydroxy and enol-glucoside were not detected.

Table B.7.6.7.3-3: Overview of European residue dat a for spirotetramat and its metabolites in cucumber used 4 times with application rates of 0.0 76 kg a.s./ha (residues are calculated as spirotetramat equivalent):

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330

Greenhouse trials

Cucumber / OD 100 Leichlingen,

Germany, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 <0.01

0.02 0.02 0.02 <0.01 <0.01 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012

0.017 0.017 0.023 0.013 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.054

0.069 0.069 0.075 0.055 <0.054 Cucumber / OD 100 Santa

Croce Camerina, Italy, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 <0.01

0.02 0.03 0.01 <0.01 <0.01 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012

0.012 0.015 0.017 0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.054

0.064 0.077 0.059 <0.054 <0.054 Cucumber / OD 100 Viladecans,

Spain, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 <0.01

0.04 0.03 0.02 <0.01 <0.01 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012

0.020 0.020 0.018 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.054

0.092 0.082 0.070 <0.054 <0.054

### - 97 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330

Cucumber / OD 100 Aronas,

Greece, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 <0.01

0.03 0.05 0.02 0.02 0.01 <0.012

0.022 0.016 <0.012 <0.012 <0.012 <0.012

0.022 0.020 0.022 0.015 0.013 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.054

0.094 0.106 0.074 0.067 0.055 Cucumber / OD 100 Leichlingen,

Germany, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 0.02

0.05 0.05 0.03 0.02 <0.01 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.019

0.024 0.019 0.015 0.020 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.071

0.106 0.101 0.077 0.072 <0.054 Cucumber / OD 100 RMolfetta

(Bari), Italy, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 <0.01

0.01 0.01 <0.01 <0.01 <0.01 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012

0.026 0.015 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.054

0.068 0.057 <0.054 <0.054 <0.054 Cucumber / OD 100 Roquetas

de Mar, Spain, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 6 7 <0.01

0.02 <0.01 <0.01 <0.01 <0.01 <0.012

0.019 0.012 <0.012 <0.012 <0.012 0.013

0.038 0.039 0.015 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.055

0.097 0.081 0.057 <0.054 <0.054 Cucumber / OD 100 Esovalta,

Greece, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 <0.01

0.04 0.01 <0.01 <0.01 <0.01 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012

0.048 0.021 0.013 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.054

0.120 0.063 <0.054 <0.054 <0.054 Field trials – Southern Europe

Cucumber / OD 100 Brenes,

Spain, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 6 7 <0.01

0.04 0.02 0.02 0.01 0.01 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012

0.018 0.015 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.054

0.090 0.067 0.064 <0.054 <0.054 Cucumber / OD 100 Malgrat de

Mar, Spain, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 6 7 <0.01

<0.01 <0.01 <0.01 <0.01 <0.01 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.054

<0.054 <0.054 <0.054 <0.054 <0.054 Cucumber / OD 100 Zapponeta

Foggia, Italy, 2004 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 <0.01

0.02 0.01 <0.01 <0.01 <0.01 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012

0.033 0.015 0.013 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.054

0.085 0.057 <0.054 <0.054 <0.054 Cucumber / OD 150 Alginet,

Spain, 2005 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 6 7 <0.01

0.03 0.02 0.02 <0.01 <0.01 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.054

0.074 0.064 0.064 <0.054 <0.054

### - 98 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330

Cucumber / OD 150 Malgrat de

Mar, Spain, 2005 fruit

fruit fruit fruit 0

3 5 7 <0.01

<0.01 <0.01 <0.01 <0.012

<0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.054

<0.054 <0.054 <0.054 Cucumber / OD 150 Vittoria,

Italy, 2005 fruit

fruit fruit fruit 0

3 5 7 0.01

<0.01 <0.01 <0.01 0.017

<0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 0.059

<0.054 <0.054 <0.054 Cucumber / OD 150 Zapponeta,

Italy, 2005 fruit

fruit fruit fruit fruit fruit 0*

0 1 3 5 7 0.03

0.06 0.07 0.06 0.05 0.03 0.021

0.035 0.025 0.027 0.020 0.019 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.083

0.127 0.127 0.119 0.102 0.081



### For the calculation of the MRL proposal, both of th e prescribed methods I and II have been used spirotetramat in cucumber (based on data obtained f rom trials from southern Europe and greenhouse):

MRL-calculation based on data obtained from the Sou thern Region (field): Individual data points for cucumber are: <0.054, <0.054, <0.054, <0.054, 0.064, 0.064, 0.119 mg/kg Mean residue: 0.066 mg/kg; standard deviation: 0.02 4 mg/kg STMR: 0.055 mg/kg Highest residue: 0.119 mg/kg Method I: R max 

### = 0.147 mg/kg Method II: R ber 

### = 0.128 mg/kg Based on the data available for cucumber in souther n Europe, a MRL of 0.2 mg/kg can be proposed.

MRL-calculation based on data obtained from the gre enhouse trials: Individual data points for cucumber are: <0.054, <0.054, 0.057, 0.059, 0.070, 0.074, 0.075, 0.077 mg/kg Mean residue: 0.065 mg/kg; standard deviation: 0.01 0 STMR: 0.065 mg/kg Highest residue: 0.077 mg/kg Method I: R max 

### = 0.096 mg/kg Method II: R ber 

### = 0.150 mg/kg Based on the data available for cucumber in greenho use, a MRL of 0.2 mg/kg can be proposed. Conclusion: 15 trials were carried out in greenhouse and southe rn Europe regions during 2004 and 2005 (7 field tri als and 8 trials in glasshouses). Spirotetramat is not intended to be used as an outdoor crop in northern Europe, therefore supervised outdoor residue trials were ca rried out in Southern European regions only. There was no significant difference between the residues in p epper grown in southern Europe and in glasshouses. Based on the submitted supervised residue trials a MRL of 0.2 mg/kg can be proposed. Comments (RMS): The residue trials in glasshouse were all performed within one season. But with respect to the protect ed cultivation of cucumber, the weather conditions in different saisons should not influence the outcome of the residue trials and the consumer risk asessment.

### - 99 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

B.7.6.7.4 Melons

Spirotetramat is applied for the use in melon again st aphids, whiteflies and mites. The critical Europ ean GAPs for the greenhouse and field uses of spirotetr amat in melon are summarised in Table 6.3.1.12-1. Table B.7.6.7.4-1: GAP for residue situation in me lons

North or South of EU Indoor or

outdoor Number of

applications Mode of

application Growth stage at

last application Application rate expressed

under the relevant unit PHI (d) EU-S F 4 Spray BBCH 87 0.072 g a.s./ha 3 EU-N/S G 4 Spray BBCH 87 0.072 kg a.s./ha 3



### Reference: Determination of the Residues of BYI08330 in/on Mel on after Spraying of BYI08330 (100 OD) in the Greenhouse in Italy, Spain , Southern France and Portugal Author(s), year: Cavaille C.; 2006 Report/Doc. number: RA-2128/04, including trials no . R 2004 0836/6, R 2004 0837/4, R 2004 0838/2, R 2004 0839/0, R 2004 0840/4, R 2004 0841/2, R 2004 0 881/1, R 2004 0883/0 M-259446-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the Residues of BYI08330 in/on Mel on after Spraying of BYI08330 (100 OD) in the Field in Italy, Spain and Greece Author(s), year: Cavaille C.; 2005 Report/Doc. number: RA-2129/04, including trials no . R 2004 0842/0, R 2004 0843/9, R 2004 0844/7, R 2004 0845/5 M-259449-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the Residues of BYI08330 in/on Mel on after Spraying of BYI08330 (150 OD) in the Field in Greece, Spain, Po rtugal and Italy Author(s), year: Cavaille C.; 2005 Report/Doc. number: RA-2042/05, including trials no . R 2005 0230/3, R 2005 0231/1, R 2005 0233/8, R 2005 0234/6, R 2005 0717/8 M-268388-02-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Experimental design: For the magnitude of residues of spirotetramat and its metabolites BYI 08330-enol, BYI 08330-ketohydro xy, BYI 08330-mono-hydroxy and BYI 08330-enol-Glc in me lons 9 trials in southern Europe (Italy, Spain, Gre ece and Portugal) and 8 trials under glasshouse conditi ons were performed in 2004 and 2005. All trials wer e

### - 100 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

carried out with oil based dispersion concentrates containing 100 and 150 g a.s./L respectively. Spirotetramat was used four times in application ra tes of 72 g a.s./ha and spray volumes between 600 a nd 1000 L/ha. An overview on the supervised residue tr ials conducted with BYI 08330 100 OD formulation is given in Table B.7.6.7.4-2 Table B.7.6.7.4-2: Overview on European residue tr ials with spirotetramat in melons

Location Formulation No. of trials Year Use rate

(g as/ha) Water volume No of appl. Spray interval

(days)

Greenhouse OD 100 8 2004 72 600-1000 L/ha 4 6-7 Field S-EU OD 100 4 2004 72 500-750 L/ha 4 6-7 Field S-EU OD 150 5 2005 72 600-1000 L/ha 4 7-10



### The last applications were carried out at growth st age between BBCH 79 and BBCH 89. Samples were taken before the last application, 0, 1, 3, 5-6 and 7 day s after the last application. All samples were stored deep frozen within 24 hours after sampling. The time intervals between date of deep-freezing and the last extraction ranged from 3 93 to 455 days for the trials carried out in 2004 a nd 82- 122 days for the residue trials from 2005. Analytical method used in all studies: Residues of spirotetramat and its metabolites BYI 0 8330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and BYI 08330-enol-Glc in melon fruit, pulp and peel were determined by HPLC-ESI-MS/MS according to method 00857. The limit of quantification (LOQ, defined as the lowest validated fortificatio n level) was 0.01 mg/kg for spirotetramat, 0.012 mg/kg for its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and 0.008 mg/kg for BYI 08330-enol-Glc in/o n melon fruits, pulp and peel (all metabolites calc ulated as spirotetramat equivalent). The mean procedural recoveries at the fortification levels of 0.01 to 1.0 mg/kg f or spirotetramat and its four metabolites ranged between 85 and 108 % and RSD < 2 0%; these results indicate that the methods used were suitable for this analysis. Findings: A detailed summary of the residue results is given in Appendix I m. 8 supervised residue trials with spirotetramat in m elon were performed in glasshouse in 2004 and altog ether 9 trials were carried out in southern Europe in 200 4 and 2005. The total residues of spirotetramat in melons (whole fruit) grown in the greenhouse ranged betwee n <0.054 and 0.00,057 mg/kg. In melons from 9 field trials in southern Europe total residues of <0.054 to 0.088 mg/kg were determined. No residues were detected in melon pulp (total residue <0.054 mg/kg) . In melon peel the total residue of spirotetramat ranged between <0,054 and 0.165 mg/kg. All trials were performed according the intended Eu ropean GAPs. An overview of the residue data is reported in the table below.The residue data used f or the evaluation are marked in bold. The total residue of BYI08330 in melon peel from th e remaining trials collected at the PHI of 3 days a fter 4 applications is composed of spirotetramat and/or th e enol metabolite; except melon fruit, pulp and pee l from trials R 2005 0230/3. In this trial the total resid ues of spirotetramat was mainly composed of BYI0833 0- monohydroxy.

### - 101 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.6.7.4-3: Overview of European residue dat a for spirotetramat and its metabolites in melon used 4 times with application rates of 0.076 kg a.s ./ha (residues are calculated as spirotetramat equivalent):

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330

Greenhouse trials

Melon OD 100 Molfetta,

Italy, 2004 fruit

fruit fruit fruit pulp peel fruit pulp peel fruit 0*

0 1 3 3 3 5 5 5 7 0.01

0.02 0.02 0.01 <0.01 0.05 0.02 <0.01 0.02 0.02 <0.012

<0.012 <0.012 <0.012 <0.012 0.019 <0.012 <0.012 0.015 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.054

0.064 0.064 <0.054 <0.054 0.101 0.064 <0.054 0.067 0.064 Melon OD 100 Sanlucar de

Bda (Monte Algaida), Spain, 2004 fruit

fruit fruit fruit pulp peel fruit pulp peel fruit 0*

0 1 3 3 3 5 5 5 7 <0.01

0.02 0.02 <0.01 <0.01 0.01 <0.01 <0.01 0.02 <0.01 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.021 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.015 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.054

0.064 0.064 <0.054 <0.054 <0.054 <0.054 <0.054 0.076 <0.054 Melon OD 100 Montfavet,

S-France, 2004 fruit

fruit fruit fruit pulp peel fruit pulp peel fruit 0*

0 1 3 3 3 6 6 6 7 <0.01

<0.01 <0.01 0.01 <0.01 0.02 <0.01 <0.01 0.02 <0.01 <0.012

<0.012 <0.012 0.014 <0.012 0.027 <0.012 <0.012 0.024 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.054

<0.054 <0.054 0.056 <0.054 0.079 <0.054 <0.054 0.076 <0.054 Melon OD 100 Torres

Vedras, Portugal, 2004 fruit

fruit fruit fruit pulp peel fruit pulp peel fruit 0*

0 1 3 3 3 5 5 5 7 <0.01

0.01 0.01 0.01 <0.01 0.04 0.01 <0.01 0.03 0.01 <0.012

<0.012 <0.012 <0.012 <0.012 0.017 <0.012 <0.012 0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 0.015 0.012 <0.012 0.029 <0.012 <0.012 0.027 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.054

<0.054 0.057 <0.054 <0.054 0.106 <0.054 <0.054 0.089 <0.054 Melon OD 100 Freiria,

Portugal, 2004 fruit

fruit fruit fruit pulp peel fruit pulp peel fruit 0*

0 1 3 3 3 5 5 5 7 <0.01

<0.01 <0.01 <0.01 <0.01 <0.01 0.01 <0.01 0.02 0.01 <0.012

<0.012 <0.012 <0.012 <0.012 0.012 <0.012 <0.012 0.020 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.054

<0.054 <0.054 <0.054 <0.054 <0.054 <0.054 <0.054 0.072 <0.054

### - 102 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330

Melon OD 100 Manfredoni

a (Fg), Italy, 2004 fruit

fruit fruit fruit pulp peel fruit pulp peel fruit 0*

0 1 3 3 3 5 5 5 7 <0.01

<0.01 <0.01 <0.01 <0.01 0.01 <0.01 <0.01 0.02 <0.01 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.013 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.054

<0.054 <0.054 <0.054 <0.054 <0.054 <0.054 <0.054 0.065 <0.054 Melon OD 100 Los

Palacios Sevilla, Spain, 2004 fruit

fruit fruit fruit pulp peel fruit pulp peel fruit 0*

0 1 3 3 3 4 4 4 7 <0.01

<0.01 <0.01 <0.01 <0.01 0.01 <0.01 <0.01 0.01 0.01 0.012

0.017 0.019 0.015 <0.012 0.022 <0.012 <0.012 0.015 0.019 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.054

0.059 0.061 0.057 <0.054 0.064 <0.054 <0.054 0.057 0.061 Melon OD 100 Vacquiers,

France, 2004 fruit

fruit fruit fruit pulp peel fruit pulp peel fruit 0*

0 1 3 3 3 5 5 5 7 <0.01

<0.01 <0.01 <0.01 <0.01 0.01 <0.01 <0.01 <0.01 <0.01 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.054

<0.054 <0.054 <0.054 <0.054 <0.054 <0.054 <0.054 <0.054 <0.054 Field trials – Southern Europe

Melon OD 100 Andria

(Bari), Italy, 2004 fruit

fruit fruit fruit pulp peel fruit fruit pulp peel 0*

0 1 3 3 3 5 7 7 7 0.02

0.05 0.05 0.04 <0.01 0.08 0.04 0.03 <0.01 0.10 <0.012

<0.012 0.014 <0.012 <0.012 0.021 <0.012 <0.012 <0.012 0.025 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 0.064

0.094 0.096 0.084 <0.054 0.133 0.084 0.074 <0.054 0.157 Melon OD 100 Gava

(Barcelona), Spain, 2004 fruit

fruit pulp peel fruit fruit pulp peel 1

3 3 3 4 7 7 7 <0.01

<0.01 <0.01 0.02 <0.01 <0.01 <0.01 <0.01 <0.012

<0.012 <0.012 0.026 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.054

<0.054 <0.054 0.078 <0.054 <0.054 <0.054 <0.054

### - 103 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330

Melon OD 100 Alginet,

Spain, 2004 fruit

fruit fruit fruit pulp peel fruit fruit pulp peel 0*

0 1 3 3 3 6 7 7 7 0.02

0.03 0.02 0.02 <0.01 0.06 0.02 0.01 <0.01 0.03 0.025

0.043 0.027 0.036 <0.012 0.073 0.026 0.021 <0.012 0.041 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 0.077

0.105 0.079 0.088 <0.054 0.165 0.078 0.063 <0.054 0.103 Melon OD 100 Aronas,

Greece, 2004 fruit

fruit fruit fruit pulp peel fruit fruit pulp peel 0

0 1 3 3 3 5 7 7 7 <0.01

0.01 0.02 0.01 <0.01 0.01 <0.01 <0.01 <0.01 0.01 <0.012

0.019 0.020 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.054

0.061 0.072 <0.054 <0.054 <0.054 <0.054 <0.054 <0.054 <0.054 Melon OD 150 AronasKaterini, Greece, 2005 fruit

fruit pulp peel fruit pulp peel fruit pulp peel 0

3 3 3 5 5 5 7 7 7 0.01

<0.01 <0.01 0.02 <0.01 <0.01 0.02 <0.01 <0.01 <0.01 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.049

0.037 0.033 0.032 0.023 0.022 0.028 0.031 0.022 0.019 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 0.091

0.079 0.075 0.084 0.065 0.064 0.080 0.073 0.064 0.061 Melon OD 150 Gava

(Barcelona), Spain, 2005 fruit

fruit pulp peel fruit pulp peel fruit pulp peel 0

3 3 3 5 5 5 7 7 7 <0.01

<0.01 <0.01 0.03 <0.01 <0.01 0.02 <0.01 <0.01 0.02 0.014

0.014 <0.012 0.041 <0.012 <0.012 0.029 <0.012 <0.012 0.015 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 0.056

0.056 <0.054 0.103 <0.054 <0.054 0.081 <0.054 <0.054 0.067 Melon OD 150 Aldeia

Gavinha, Portugal, 2005 fruit

fruit fruit pulp peel fruit pulp peel fruit pulp peel fruit pulp peel 0*

0 1 1 1 3 3 3 4 4 4 7 7 7 <0.01

<0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.012

0.016 0.021 <0.012 0.041 0.017 <0.012 0.036 0.015 <0.012 0.031 0.012 <0.012 0.023 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.054

0.058 0.063 <0.054 0.083 0.059 <0.054 0.078 0.057 <0.054 0.073 <0.054 <0.054 0.065

### - 104 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330

Melon OD 150 Licodia

Eubea (CT.), Italy, 2005 fruit

fruit fruit fruit pulp peel fruit pulp peel fruit pulp peel 0}

0 1 3 3 3 5 5 5 7 7 7 <0.01

0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.012

<0.012 <0.012 <0.012 <0.012 0.031 <0.012 <0.012 0.016 <0.012 <0.012 0.015 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.054

<0.054 <0.054 <0.054 <0.054 0.073 <0.054 <0.054 0.058 <0.054 <0.054 0.057 Melon OD 150 Alginet,

Spain, 2005 fruit

fruit fruit fruit pulp peel fruit pulp peel fruit pulp peel 0*

0 1 3 3 3 4 4 4 7 7 7 <0.01

<0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.01 <0.012

0.013 <0.012 <0.012 <0.012 0.018 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.054

0.055 <0.054 <0.054 <0.054 0.060 <0.054 <0.054 <0.054 <0.054 <0.054 <0.054



### For the calculation of the MRL proposal, both of th e prescribed methods I and II have been used spirotetramat in melon (based on data obtained from trials from southern Europe and greenhouse):

MRL-calculation based on data obtained from the Sou thern Region (field): Individual data points for melon are: <0.054, <0.054, <0.054, <0.054, 0.056, 0.059, 0.079 , 0.084, 0.088 mg/kg Mean residue: 0.065 mg/kg; standard deviation: 0.01 5 mg/kg STMR: 0.056 mg/kg Highest residue: 0.088 mg/kg Method I: R max 

### = 0.109 mg/kg Method II: R ber 

### = 0.163 mg/kg Based on the data available for melon in southern E urope, a MRL of 0.2 mg/kg can be proposed.

MRL-calculation based on data obtained from the gre enhouse trials: Individual data points for melon are: <0.054,< 0.054, <0.054, <0.054, <0.054, <0.054, 0.0 56, 0.057 mg/kg Mean residue: 0.055 mg/kg; standard deviation: 0.00 1 STMR: 0.054 mg/kg Highest residue: 0.057 mg/kg Method I: R max 

### = 0.058 mg/kg Method II: R ber 

### = 0.111 mg/kg Based on the data available for melon in greenhouse , a MRL of 0.2 mg/kg can be proposed. Conclusion: 17 trials were carried out in greenhouse and southe rn Europe regions during 2004 and 2005 (7 field tri als and 8 trials in glasshouses). Spirotetramat is not intended to be used on melons as an outdoor crop in northern Europe, therefore supervised outdoor resid ue trials were carried out in Southern European reg ions

### - 105 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

only. The residues in melons grown in southern Euro pe were slightly higher than those which were grown in glasshouses. Based on the submitted supervised resi due trials a MRL of 0.2 mg/kg can be proposed. Comments (RMS): The residue trials in glasshouse were all performed within one season. But with respect to the protect ed cultivation of cucumber, the weather conditions in different saisons should not influence the outcome of the residue trials and the consumer risk asessment.

B.7.6.8 Brassica vegetables

B.7.6.8.1 Flowering brassica

Spirotetramat is applied for control of aphids in b rassica vegetables. The critical European GAPs for the greenhouse and field uses of spirotetramat in flowe ring brassica are summarised in Table B.7.6.8-1. Table B.7.6.8-1: GAP for residue situation in flow ering brassica

North or South of EU Indoor or

outdoor Number of

applications Mode of

application Growth stage at

last application Application rate expressed

under the relevant unit PHI (d) EU-N F 2 Spray BBCH 79 0.072 g a.s./ha 3 EU-S F 2 Spray BBCH 79 0.072 g a.s./ha 3



### Reference: Determination of the residues of BYI08330 in/on bro ccoli after spraying of BYI08330 (100 OD) in the field in Germany and Unite d Kingdom Author(s), year: Bardel P.; Freitag T.; 2005 Report/Doc. number: RA-2022/04, including trials no . R 2004 0105/1, R 2004 0108/6 M-259571-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the residues of BYI08330 in/on cau liflower after spraying of BYI08330 (100 OD) in the field in Germany and Franc e Author(s), year: Zimmer D.; Freitag T.; 2005 Report/Doc. number: RA-2023/04, including trials no . R 2004 0109/4, R 2004 0110/8 M-259580-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

### - 106 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Reference: Determination of the residues of BYI08330 in/on bro ccoli after spraying of BYI08330 (100 OD) in the field in Italy Author(s), year: Bardel P.; Freitag T.; 2006 Report/Doc. number: RA-2024/04, including trials no . R 2004 0111/6 M-259272-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the residues of BYI08330 in/on cau liflower after spraying of BYI08330 (100 OD) in the field in France Author(s), year: Zimmer D.; Freitag T.; 2005 Report/Doc. number: RA-2025/04, including trials no . R 2004 0112/4 M-258975-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the residues of BYI08330 in/on bro ccoli and cauliflower after spraying of BYI08330 (150 OD) in the field in Germany, northern France, and United Kingdom Author(s), year: Freitag T., Wieland K. 2006 Report/Doc. number: RA-2062/05, including trials no . R 2005 0363/6, R 2005 0364/4, R 2005 0365/2, R 2005 1017/9, R 2005 1047/0 M-275226-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the residues of BYI08330 in/on bro ccoli and cauliflower after spraying of BYI08330 (150 OD) in the field in Italy and Spain Author(s), year: Freitag T., Wieland K., 2006 Report/Doc. number: RA-2063/05, including trials no . R 2005 036/1, R 2005 0362/8 M-275233-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Experimental design: The magnitude of residues of spirotetramat and its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-mono-hydroxy and BYI 08330-enol-Glc in/on bro ccoli and cauliflower harvested following the

### - 107 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

treatment with BYI 08330 formulations (100 OD, 150 OD) under field conditions was determined in northe rn (Germany, UK and N-France) and southern Europe (Ita ly, S-France and Spain) in 2004 and 2005. Cauliflower is classified as major crops in norther n Europe and as minor crop in southern Europe. For extrapolation to the whole group of flowering brass ica, a minimum of 4 trials on cauliflower and 4 tri als on broccoli are required. In northern Europe 4 trials on cauliflower and 5 trials on broccoli were perfor med. For southern Europe two trials on broccoli and two tria ls on cauliflower were carried out. An overview on the supervised residue trials conducted with different formulations of spirotetramat is given in Table B.7 .6.8.1-2.

Table B.7.6.8.1-2: Overview on European residue tri als with BYI08330 in flowering brassica

Location Formulation No. of trials Year Use rate

(g as/ha) Water volume No of appl. Spray interval

(days)

Field N-EU OD 100 4 2004 72-77 300-323 3 7 Field N-EU OD 150 4 2005 72 500-600 2-3 14-21 Field S-EU OD 100 2 2004 72 500,800 3 7 Field S-EU OD 150 2 2005 72 600 3 14



### In 2004, 3 spray applications of spirotetramat were performed with a spray interval of 7 days. Samples were taken before the last application, 0, 3, 7, 13-14 a nd 21 days after the last application. The notifier stated that due to new results from biological trials the criti cal GAP changed: The number of applications was cha nged from 3 to 2 and the spray interval from 7 days to 1 4 days. Therefore the residue trials from 2005 were performed with 3 applications and a spray interval of 14 days. Samples were taken 0-21 days after the last application. To cover the use pattern with two appl ications additional samples were taken directly aft er the second application and 3 days later. In trial R 200 5 1047/0 the 3 rd 

### application was delayed for one week, because the plants grew slowly due to cold weather conditions. The last application was carried out at growth stag e BBCH 41 – 49. All samples were stored deep frozen within 24 hours after sampling. The time intervals between date of deep-freezing and the last extraction ranged from 3 4 to 283 days. Analytical method used in all studies: Residues of spirotetramat and its metabolites BYI 0 8330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and BYI 08330-enol-Glc were determined by H PLC-ESI-MS/MS according to method 00857. The limit of quantification (LOQ, defined as the lowest validated fortificatio n level) was 0.01 mg/kg for spirotetramat, 0.012 mg/kg for its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and 0.008 mg/kg for BYI 08330-enol-Glc in/o n flowering brassica (all metabolites were calculat ed as spirotetramat equivalent). The mean procedural recoveries at the fortification levels of 0.01 to 10.0 mg/kg for spirotetramat and its four metabolites ranged between 70 and 110 % and RSD was <20%; these results indicate that the methods used were suitable for this analysis. Findings: A detailed summary of the residue results is given in Appendix In. Nearly all residue trials for the residue behaviour of spirotetramat on cauliflower and broccoli were carried out with 3 applications per seasons. Number of applicat ions and spray interval (6-8 days instead of 14 day s) in the submitted trials carried out in 2004 are not in accordance with the intended use for flowering bra ssica. In the residue trials performed in 2005, the first spe cimens were taken directly after the 2 nd 

### application and 3 days later, therefore it was possible to compare th e residues after three and two applications. Neither the number of applications nor the time int erval between the applications seems to have any influence on the resulting residues. Residues of to tal spirotetramat in flowering brassica after 3 app lications ranged between 0.11 and 0.58 mg/kg whereas after 2 applications residues from 0.16 to 0.64 mg/kg were detected. An overview on the results of the residue data is summarized in the table below. The residue values used for evaluation are marked with bold num bers.

### - 108 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

The total residue of spirotetramat is mainly compos ed of the enol and the ketohydroxy metabolites. The parent compound and the enol-glucoside were present at lower amounts. BYI08330-monohydroxy was not detected or in traces, only.

Table B.7.6.8-3: Overview of European residue data for spirotetramat and its metabolites in flowering brassica used 2-3 times with application rates of 0 .076 kg a.s./ha (residues are calculated as spirotetramat equivalent):

crop / No of appl./ fomulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 Field trials – Northern Europe

broccoli/ 3 appl./ OD 100 Langenfeld

Germany, 2004 curd

curd curd curd curd 0*

0 3 7 13 <0.01

0.08 0.07 0.01 0.01 0.17

0.17 0.20 0.14 0.097 0.21

0.22 0.28 0.20 0.12 <0.012

<0.012 <0.012 <0.012 <0.012 0.013

0.013 0.016 0.012 0.008 0.415

0.495 0.578 0.374 0.247 broccoli/ 3 appl./ OD 100 Rollesby

United Kingdom, 2004 curd

curd curd curd curd curd 0*

0 3 7 14 21 0.01

0.24 0.09 <0.01 <0.01 <0.01 0.29

0.48 0.28 0.29 0.18 0.15 0.067

0.14 0.13 0.13 0.10 0.048 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.009

0.008 0.009 0.008 0.008 0.008 0.388

0.880 0.521 0.450 0.310 0.228 cauliflower/ 3 appl./ OD 100 Langenfeld

Germany, 2004 curd

curd curd curd curd 0*

0 3 7 13 <0.01

0.02 <0.01 <0.01 <0.01 0.074

0.033 0.055 0.019 0.013 0.20

0.24 0.34 0.28 0.14 <0.012

<0.012 <0.012 <0.012 <0.012 0.008

0.011 0.010 0.010 0.008 0.304

0.316 0.427 0.331 0.183 cauliflower/ 3 appl./ OD 100 Criquebeuf

sur Seine N-France, 2004 curd

curd curd curd curd curd 0*

0 3 7 14 21 <0.01

0.01 0.02 <0.01 <0.01 <0.01 0.035

0.079 0.077 0.14 0.15 0.12 0.034

0.048 0.046 0.069 0.061 0.076 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.008

0.008 0.008 0.008 0.008 0.008 0.099

0.157 0.163 0.239 0.241 0.226 broccoli/ 3 appl./ OD 150 Leichlingen

Germany, 2005 curd

curd curd curd curd curd curd curd -14

-11 0* 0 3 7 14 21 0.57

0.19 0.01 0.10 0.01 <0.01 <0.01 <0.01 0.25

0.24 0.073 0.26 0.14 0.18 0.89 0.092 0.10

0.18 0.074 0.17 0.13 0.15 0.047 0.038 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <o.012 <0.012 <0.008

0.019 0.011 0.008 0.021 0.032 0.011 0.011 0.940

0.641 0.180 0.550 0.313 0.384 0.169 0.163 broccoli/ 3 appl./ OD 150 Ennemain

N-France, 2005 curd

curd curd curd curd curd -14

-11 0 3 7 14 0.09

0.03 0.11 0.01 0.01 0.01 0.28

0.12 0.078 0.048 0.046 0.033 0.12

0.082 0.047 0.032 0.025 0.022 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

0.018 0.008 <0.008 <0.008 0.008 0.510

0.262 0.255 0.110 0.101 0.085 cauliflower/ 3 appl./ OD 150 Schauernheim Germany, 2005 curd

curd curd curd curd curd curd curd -14

-11 0* 0 3 7 14 21 0.01

<0.01 <0.01 0.02 0.02 0.02 0.01 <0.01 0.11

0.15 0.091 0.13 0.14 0.13 0.12 0.086 0.027

0.029 0.023 0.048 0.040 0.031 0.034 0.030 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 0.008 0.008 <0.008 0.008 0.008 0.167

0.209 0.144 0.218 0.220 0.201 0.184 0.146

### - 109 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / No of appl./ fomulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330

broccoli/ 2 appl./ OD 150 Mecklenbeuren Germany, 2005 curd

curd 0

3 0.07

0.01 0.15

0.18 0.099

0.098 <0.012

<0.012 0.008

0.008 0.339

0.308

cauliflower/ 3 appl./ OD 150 Ipswich

United Kingdom, 2005 curd

curd curd curd curd curd -21

-19 0 3 7 13 <0.01

<0.01 <0.01 <0.01 <0.01 <0.01 0.079

0.12 0.23 0.24 0.31 0.25 0.012

0.012 0.036 0.059 0.029 0.039 <0.012

0.012 <0.012 <0.012 <0.012 0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.121

0.162 0.296 0.329 0.369 0.319 Field trials – Southern Europe

broccoli/ 3 appl./ OD 100 Zapponeta

Italy, 2004 curd

curd curd curd curd 0*

0 3 7 14 0.04

0.13 0.02 0.02 0.01 0.13

0.19 0.20 0.31 0.25 0.069

0.094 0.080 0.089 0.068 <0.012

<0.012 <0.012 <0.012 <0.012 <0.008

0.008 <0.008 0.008 0.008 0.259

0.434 0.320 0.439 0.348 cauliflower/ 3 appl./ OD 100 Fenouillet

S-France, 2004 curd

curd curd curd curd curd 0*

0 3 7 14 20 <0.01

<0.01 <0.01 <0.01 <0.01 <0.01 0.075

0.095 0.077 0.13 0.13 0.11 0.067

0.078 0.081 0.10 0.074 0.067 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.008

0.008 0.008 0.008 0.008 0.008 0.172

0.203 0.188 0.260 0.234 0.207 broccoli/ 3 appl./ OD 150 Manfredoni

a Italy, 2005 curd

curd curd curd curd curd curd curd -14

-11 0* 0 3 8 14 20 0.08

0.06 0.01 0.11 0.01 0.01 0.01 <0.01 0.11

0.099 0.11 0.15 0.11 0.12 0.13 0.087 0.037

0.036 0.025 0.043 0.029 0.035 0.036 0.026 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

0.008 0.008 0.008 0.008 0.008 0.008 0.011 0.247

0.215 0.165 0.323 0.169 0.185 0.196 0.146 cauliflower/ 3 appl./ OD 150 Gava

Spain, 2005 whole pl.

whole pl. curd curd curd curd -14

-11 0* 0 3 7 1.0

0.06 0.01 0.13 0.01 <0.01 0.23

0.10 0.039 0.085 0.070 0.084 0.049

0.019 0.012 0.013 0.013 0.014 <0.012

0.012 <0.012 <0.012 <0.012 <0.012 0.008

0.008 0.008 0.013 0.008 0.010 1.299

0.199 0.081 0.253 0.113 0.130



### Cauliflower is classified as major crops in norther n Europe and as minor crop in southern Europe. For extrapolation to the whole group of flowering brass ica, a minimum of 4 trials on cauliflower and 4 tri als on broccoli are required. Hence, the number of application did not have much influence on the resulting residues, the results of the residue trials carried out with 3 applications were taking into account for MRL calculation. For the calculation of the MRL proposal, both of th e prescribed methods I and II have been used for spirotetramat in flowering brassica (based on data obtained from trials from Northern and Southern Eur ope):

MRL-calculation based on data obtained from the Nor thern Region: Individual data points for cauliflower are: 0.22, 0.241, 0.369, 0.427 mg/kg Individual data points for broccoli are: 0.11, 0.308, 0.384, 0.521, 0.578 mg/kg Mean residue: 0.351mg/kg; standard deviation: 0.149 mg/kg STMR: 0.369 mg/kg Highest residue: 0.578 mg/kg

### - 110 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Method I: R max 

### = 0.802 mg/kg Method II: R ber 

### = 0.948 mg/kg Based on the data available for flowering brassica in northern Europe, a MRL of 1 mg/kg can be proposed.

MRL-calculation based on data obtained from the Sou thern Region: Individual data points for cauliflower are: 0.196, 0.439mg/kg Individual data points for broccoli are: 0.130, 0.260mg/kg Mean residue: 0.256 mg/kg; standard deviation: 0.13 3 mg/kg STMR: 0.228 mg/kg Highest residue: 0.439 mg/kg Method I: R max 

### = 0.940 mg/kg Method II: R ber 

### = 0.789 mg/kg Based on the data available for flowering brassica in southern Europe, a MRL of 1 mg/kg can be proposed.

Conclusion: Nearly all residue trials concerning the residue be haviour of spirotetramat in flowering brassica were carried out with three applications per season. In the tria ls from 2005 the first sampling was made directly a fter the

2 nd 

### application and three days after the 2 nd 

### application. The comparison of the specimens taken after the 2 nd 

### application and the samples 3 days after the 3 rd 

### application showed comparable results; therefore t he results were taken for MRL calculation. Based on the availa ble trials on cauliflower and broccoli a MRL of 1 mg/kg for flowering brassica can be proposed. Comments (RMS): No comments.

B.7.6.8.2 Head brassica

B.7.6.8.2.1 Brussels sprouts

Spirotetramat is applied for the use in Brussels sp routs in northern Europe against aphids. The critic al European GAPs are summarised in table B.7.6.8.2.1-1

.

Table B.7.6.8.2.1-1: GAP for residue situation in Brussels sprouts

North or South of EU Indoor or

outdoor Number of

applications Mode of

application Growth stage at

last application Application rate expressed

under the relevant unit PHI (d) EU-N F 2 Spray BBCH 79 0.072 g a.s./ha 3



### Reference: Determination of the Residues of BYI08330 in/on Bru ssels Sprouts after Spraying of BYI08330 (100 OD) in the Field in Germa ny and Northern France Author(s), year: Freitag T.; Wolters A.; 2005 Report/Doc. number: RA-2039/04, including trials no . R 2004 0160/4, R 2004 0161/2, R 2004 0162/0, R 2004 0163/9 M-260437-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

### - 111 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Reference: Determination of the Residues of BYI08330 in/on Bru ssels Sprouts after Spraying of BYI08330 (150 OD) in the Field in Germa ny, Northern France and United Kingdom Author(s), year: Freitag T.; Eberhardt R. ; Wolters A.; 2006 Report/Doc. number: RA-2066/05, including trials no . R 2005 0369/5, R 2005 0370/9, R 2005 0371/7, R 2005 0372/5 M-273238-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Experimental design: In 2004 and 2005, the magnitude of residues of spir otetramat and its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-mono-hydroxy and BYI 0 8330-enol-Glc in/on Brussels sprouts harvested following the treatment with BYI 08330 formulations (100 OD, 150 OD) was determined in northern Europe (Germany, UK and N-France). In northern Europe 8 trials on Brussels sprouts wer e performed using different formulations of spirote tramat An overview on the supervised residue trials conduc ted with different formulations of spirotetramat is given in table B.7.6.8.2.1-2.

Table B.7.6.8.2.1-2: Overview on European residue trials with BYI08330 in Brussels sprouts

Location Formulation No. of trials Year Use rate

(g as/ha) Water volume No of appl. Spray interval

(days)

Field N-EU OD 100 4 2004 72 500 3 7 Field N-EU OD 150 4 2005 72 500 3 3-10



### In 2004, 3 spray applications of spirotetramat were performed with a spray interval of 7 days. Samples were taken before the last application, 0, 3, 7-8, 14 an d 21 days after the last application. The notifier stated that due to new results from biological trials the criti cal GAP changed: The number of applications was cha nged from 3 to 2 and the spray interval from 7 days to 1 4 days. Therefore the residue trials from 2005 were performed with 3 applications and a spray interval of 14 days. Samples were taken directly after the s econd application, and 3 days later (to cover the use pat tern with two applications), before and after the t hird application, 3, 7-8, 14 and 21 days after the last application. To cover the use pattern with two appl ications additional samples were taken directly after the se cond application and 3 days later. The last application was carried out at growth stag e BBCH 46 – 49. All samples were stored deep frozen within 24 hours after sampling. The time intervals between date of deep-freezing and the last extraction ranged from 6 9 to 193 days. Analytical method used in all studies: Residues of spirotetramat and its metabolites BYI 0 8330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and BYI 08330-enol-Glc were determined by H PLC-ESI-MS/MS according to method 00857. The limit of quantification (LOQ, defined as the lowest validated fortificatio n level) was 0.01 mg/kg for spirotetramat, 0.012 mg/kg for its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and 0.008 mg/kg for BYI 08330-enol-Glc in/o n Brussels sprouts (all metabolites were calculated as spirotetramat equivalent). The mean procedural recoveries at the fortification levels of 0.01 to 10.0 mg/kg for spirotetramat and its four metabolites ranged between 70 and 110 % and RSD was <20%; these results indicate that the methods used were suitable for this analysis. Findings: A detailed summary of the residue results is given in Appendix I o.

### - 112 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

All residue trials for the residue behaviour of spi rotetramat on Brussels sprouts were carried out wit h 3 applications per seasons. Number of applications an d different spray intervals in the submitted trials carried out in 2004 are not in accordance with the intended use for Brussels sprouts. In the residue trials pe rformed in 2005, the first specimens were taken directly af ter the 2 nd 

### application and 3 days later, therefore it was possible to compare the residues after three and tw o applications. Neither the number of applications nor the time int erval between the applications seemed to have an influence on the resulting residues. Residues of to tal spirotetramat in Brussels sprouts after 3 appli cations ranged between 0.089 and 0.203 mg/kg whereas after 2 applications residues from 0.092 to 0.105 mg/kg were detected. An overview on the results of the re sidue data is summarized in the table below. The re sidue values used for evaluation are marked with bold num bers. The total residue of spirotetramat is mainly compos ed of the enol and the ketohydroxy metabolites. The parent compound and the enol-glucoside were present at lower amounts. BYI08330-monohydroxy was not detected or in traces, only.

Table B.7.6.8.2.1-3: Overview of European residue d ata for spirotetramat and its metabolites in Brussels sprouts used 3 times with application rate s of 0.072 kg a.s./ha (residues are calculated as spirotetramat equivalent):

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 Field trials – northern Europe

brussels sprouts / OD 100 Hennef

Germany, 2004 sprout

sprout sprout sprout sprout 0*

0 3 7 14 0.01

0.03 0.01 0.01 0.01 0.022

0.044 0.041 0.051 0.053 0.012

0.016 0.013 0.025 0.014 <0.012

<0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.08 0.064

0.11 0.084 0.106 0.097 brussels sprouts/ OD 100 Langenfeld,

Germany, 2004 sprout

sprout sprout sprout sprout 0*

0 3 7 14 <0.01

0.01 0.01 0.01 0.01 0.012

0.018 0.021 0.035 0.041 0.012

0.013 0.012 0.018 0.017 <0.012

<0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.054

0.061 0.063 0.083 0.088

brussels sprouts/ OD 100 Criqubeuf

sur Seine N- France, 2004 sprout

sprout sprout sprout sprout sprout 0*

0 3 8 14 21 0.01

0.02 0.01 <0.01 <0.01 <0.01 0.023

0.043 0.039 0.069 0.051 0.051 0.023

0.034 0.025 0.032 0.023 0.016 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.076

0.117 0.094 0.131 0.104 0.097 brussels sprouts/ OD 100 Fontaine

L’Etalon N-France, 2004 sprout

sprout sprout sprout sprout sprou t 0*

0 3 7 14 21 <0.01

0.01 0.01 0.01 <0.01 <0.01 0.042

0.051 0.075 0.099 0.098 0.13 0.014

0.023 0.032 0.045 0.043 0.058 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.086

0.104 0.137 0.174 0.171 0.218

brussels sprouts / OD 150 WerlWestönnen Germany, 2005 sprout

sprout sprout sprout sprout sprout -14

-11 0 3 8 14 0.01

0.01 0.02 0.01 <0.01 <0.01 0.032

0.036 0.049 0.029 0.026 0.024 0.029

0.038 0.039 0.030 0.021 0.019 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.008

0.009 0.011 0.008 0.008 0.008 0.091

0.105 0.131 0.089 0.077 0.073 brussels sprouts / OD 150 Criquebeuf

sur Seine N-France, 2005 sprout

sprout sprout sprout sprout sprout -14

-11 0 3 7 14 0.01

0.01 0.01 0.01 <0.01 0.01 0.043

0.041 0.045 0.035 0.041 0.041 0.027

0.023 0.020 0.020 0.017 0.018 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.008

0.008 0.008 0.008 0.008 0.008 0.100

0.094 0.095 0.085 0.088 0.089

### - 113 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330

brussels sprouts / OD 150 Bornheim

Germany, 2005 sprout

sprout sprout sprout sprout sprout sprout sprout -14

-11 0* 0 3 7 14 21 0.01

0.01 0.02 <0.01 0.01 0.01 0.01 0.01 0.030

0.033 0.071 0.057 0.057 0.064 0.064 0.060 0.020

0.025 0.046 0.023 0.046 0.034 0.039 0.027 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

0.012 0.008 0.008 0.008 <0.008 0.008 0.030 0.080

0.092 0.157 0.110 0.133 0.128 0.133 0.139

brussels sprouts / OD 150 Saxmundham United Kingdom, 2005 sprout

sprout sprout sprout sprout sprout sprout sprout -15

-11 0* 0 3 7 14 21 0.02

0.01 0.02 <0.01 0.01 0.01 0.01 <0.01 0.032

0.033 0.059 0.044 0.053 0.068 0.062 0.065 0.012

0.012 0.012 0.012 0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.008

0.008 <0.008 0.008 <0.008 <0.008 <0.008 <0.008 0.084

0.075 0.111 0.086 0.095 0.110 0.104 0.107



### Hence, the number of applications did not have much influence on the resulting residues the results of the residue trials carried out with 3 applications were taking into account for MRL calculation. For the calculation of the MRL proposal, both of th e prescribed methods I and II have been used for spirotetramat in Brussels sprouts (based on data ob tained from trials from Northern Europe):

MRL-calculation based on data obtained from the nor thern region: Individual data points for Brussels sprouts are: 0.088, 0.089, 0.089, 0.106, 0.11, 0.131, 0.139, 0.2 18 mg/kg Mean residue: 0.121 mg/kg; standard deviation: 0.04 4 STMR: 0.108 mg/kg Highest residue: 0.218 mg/kg Method I: R max 

### = 0.260 mg/kg Method II: R ber 

### = 0.275 mg/kg Based on the data available for Brussels sprouts in northern Europe, a MRL of 0.3 mg/kg can be proposed. Conclusion: Brussels sprouts are applied only for the use of sp irotetramat in northern Europe. 8 supervised residu e trials were submitted to support this use. All trials were carried out with 3 applications. In 2005, to cover the GAPs with three and four applications, the first samplin g was made directly after the second application an d the next samples were taken three days after the second application (according the intended use). The resu lts from these trials are well corresponding to the spe cimens taken from the other trials carried out with 3 applications. Therefore the trials conducted with 3 applications were considered in the MRL-calculatio n. The residues of spirotetramat and its metabolites on Br ussels sprouts ranged between 0.088 – 0.218 mg/kg. The data is sufficient to propose an EU MRL and a MRL of 0.3 mg/kg can be proposed. Comments (RMS): No comments.

B.7.6.8.2.2 Head cabbage

Spirotetramat is applied for control of aphids in h ead cabbage. The critical European GAPs for the greenhouse and field uses of spirotetramat on head cabbage are summarised in Table B.7.6.8.2.2-1.

### - 114 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.6.8.2.2-1: GAP for residue situation in head cabbage

North or South of EU Indoor or

outdoor Number of

applications Mode of

application Growth stage at

last application Application rate expressed

under the relevant unit PHI (d) EU-N F 2 Spray BBCH 79 0.072 g a.s./ha 3 EU-S F 2 Spray BBCH 79 0.072 g a.s./ha 3



### Reference: Determination of the Residues of BYI08330 in/on Rou nd Cabbage, Red Cabbage and Savoy Cabbage after spraying of BYI0833 0 (100 OD) in the Field in Germany, United Kingdom and Northern Franc e Author(s), year: Freitag T.; Wolters A.; 2005 Report/Doc. number: RA-2037/04, including trials no . R 2004 0152/3, R 2004 0156/6, R 2004 0157/4 M-260141-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the Residues of BYI08330 in/on Red Cabbage and Round Cabbage after Spraying of BYI08330 (100 OD) in the Field in Spain and Italy Author(s), year: Freitag T.; Behn U.; 2005 Report/Doc. number: RA-2038/04, including trials no . R 2004 0158/2, R 2004 0159/0 M-260014-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the residues of BYI08330 in/on red cabbage, round cabbage and Savoy cabbage after spraying of BYI0833 0 (150 OD) in the field in Northern-France and Germany Author(s), year: Ballesteros; Gateaud L.; 2006 Report/Doc. number: RA-2060/05, including trials no . R 2005 0352/0, R 2005 0353/9, R 2005 0354/7, R 2005 0355/5, R 2005 0356/3, R 2005 0357/1, R 2005 0 359/8 M-272557-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

### - 115 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Reference: Determination of the residues of BYI08330 in/on red cabbage and round cabbage after spraying of BYI08330 (150 OD) in the field in Italy and Spain Author(s), year: Ballesteros; Gateaud L.; 2006 Report/Doc. number: RA-2061/05, including trials no . R 2005 0350/4, R 2005 0351/2 M-272570-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Experimental design: The magnitude of residues of spirotetramat and its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-mono-hydroxy and BYI 08330-enol-Glc in/on hea d cabbage following the treatment with BYI 08330 formulations (100 OD, 150 OD) under field condition s was determined in 2004 and 2005. 10 supervised residue trials were performed in northern (Germany, UK and N-France) and 4 trials were carried out in southern Europe (Italy, S-France and Spain). An overview on the supervised residue trials conduc ted with different formulations of spirotetramat is given in Table B.7.6.8.2.2-2.

Table B.7.6.8.2.2-2: Overview on European residue trials with BYI08330 in head cabbage

Location Formulation No. of trials Year Use rate

(g as/ha) Water volume No of appl. Spray interval

(days)

Field N-EU OD 100 3 2004 72 500-600 3 6-8 Field N-EU OD 150 7 2005 72 500-600 2-3 14 Field S-EU OD 100 2 2004 72 600, 800 3 7 Field S-EU OD 150 2 2005 72 500-800 3 14-22



### In the residue trials 2004, 3 spray applications of spirotetramat were performed with a spray interval of 7 days. Samples were taken before the last applicatio n, 0, 3, 6-7, 13-14 and 20-23 days after the last application. The notifier stated that due to new re sults from biological trials the critical GAP chang ed: The number of applications was lowered from 3 to 2 and the spray interval extended from 7 days to 14 days. The residue trials from 2005 were performed with 3 appl ications and a spray interval of 14 days. Samples w ere taken 0-21 days after the last application and to c over the use pattern with two applications, additio nal samples were taken directly after the second applic ation and 3 days later. The last application was carried out at growth stag e BBCH 45 – 49. All samples were stored deep frozen within 24 hours after sampling. The time intervals between date of deep-freezing and the last extraction ranged from 3 5 to 268 days.

Analytical method used in all studies: Residues of spirotetramat and its metabolites BYI 0 8330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and BYI 08330-enol-Glc in red, white and Sa voy cabbage were determined by HPLC-ESI-MS/MS according to method 00857. The limit of quantification (LOQ, defined as the lowest validated fortificatio n level) was 0.01 mg/kg for spirotetramat, 0.012 mg/kg for its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and 0.008 mg/kg for BYI 08330-enol-Glc in/o n head cabbages (all metabolites were calculated as spirotetramat). The mean procedural recoveries at the fortification levels of 0.01 to 5.0 mg/kg f or spirotetramat and its four metabolites ranged between 70 and 110 % and RSD was <20%; these results indicate that the methods used were suitable for this analysis.

### - 116 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Findings: A detailed summary of the residue results is given in Appendix I p. The residue trials for the residue behaviour of spi rotetramat on red, white and Savoy cabbage were car ried out with 3 applications per seasons. Number of appl ications and spray interval (6-8 days instead of 14 days) in the submitted trials carried out in 2004 are not in accordance with the intended use for flowering brassica. In the residue trials performed in 2005, the first specimens were taken directly after the 2 nd 

### application and 3 days later, therefore it was possible to compare th e residues after three and two applications. Neither the number of applications nor the time int erval between the applications seemed to have an influence on the resulting residues. Residues of to tal spirotetramat in head cabbages after 3 applicat ions ranged between 0.067 and 0.261 mg/kg whereas after 2 applications residues between 0.060 and 0.478 mg/kg were detected. An overview on the results of the residue data is summarized in the table below. The residue values used for evaluation are marked with bold numbers. The total residue of spirotetramat is mainly compos ed of the enol and the ketohydroxy metabolites. The parent compound and the enol-glucoside were present at lower amounts. BYI08330-monohydroxy was not detected or in traces, only.

Table B.7.6.8.2.2-3: Overview of European residue data for spirotetramat and its metabolites in head cabbage used 2-3 times with application rates of 0. 072 kg a.s./ha (residues are calculated as spirotetramat equivalent):

crop / fomulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 Field trials – Northern Europe

round cabbage OD 100 Langenfeld,

Germany, 2004 head

head head head head 0*

0 3 7 14 0.01

0.13 0.01 0.01 <0.01 0.024

0.025 0.032 0.037 0.018 0.024

0.022 0.023 0.030 0.025 <0.012

<0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 0.078

0.197 0.085 0.097 0.073 red cabbage OD 100 Frithville,

United Kingdom, 2004 head

head head head head head 0*

0 3 6 14 20 0.01

0.04 0.01 0.01 <0.01 <0.01 0.065

0.062 0.060 0.059 0.062 0.059 0.013

0.012 0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0,012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.108

0.134 0.102 0.101 0.104 0.101 Savoy cabbage OD 100 Faverolles

N-France, 2004 head

head head head head head 0*

0 3 7 14 21 <0.01

0.04 0.01 <0.01 <0.01 <0.01 0.012

0.045 0.017 0.012 0.012 0.012 0.035

0.070 0.044 0.014 0.012 0.013 <0.012

<0.012 <0.012 <0.012 <0.012 <0,012 <0.008

0.008 0.008 <0.008 <0.008 <0.008 0.077

0.175 0.091 0.056 <0.054 0.055 red cabbage OD 150 Dury

N-France, 2005 head

head head head head head head head -14

-11 0* 0 3 7 14 21 <0.01

0.012 <0.01 0.022 0.010 <0.01 <0.01 <0.01 0.014

0.019 0.014 0.020 0.025 0.025 0.017 0.024 <0.012

<0.012 <0.012 <0.012 <0.012 <0,012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0,012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 0.056

0.063 0.056 0.074 0.067 0.067 0.059 0.066 red cabbage OD 150 Burscheid

Germany, 2005 head

head head head head head -14

-11 0 3 7 14 0.036

<0.01 0.038 <0.01 <0.01 <0.01 0.01

0.095 0.11 0.092 0.090 0.072 <0.012

<0.012 <0.012 <0.012 <0.012 <0,012 <0.012

<0.012 <0.012 <0.012 <0.012 <0,012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.078

0.137 0.180 0.134 0.132 0.114

### - 117 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / fomulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330

round cabbage OD 150 Leichlingen

Germany, 2005 head

head head head head head head head -14

-11 0* 0 3 7 14 21 <0.01

<0.01 <0.01 0.057 0.011 <0.01 <0.01 <0.01 0.032

0.052 0.040 0.058 0.061 0.062 0.053 0.037 0.044

0.067 0.071 0.087 0.094 0.093 0.099 0.074 <0.012

<0.012 <0.012 <0.012 <0.012 <0,012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 0.106

0.149 0.141 0.222 0.186 0.185 0.182 0.141 round cabbage OD 150 WerlWestönnen Germany, 2005 head

head head head head head -14

-11 0 3 8 14 <0.01

<0.01 <0.01 <0.01< 0.01 <0.01 0.036

0.035 0.037 0.024 0.032 0.026 0.021

0.022 0.021 0.014 0.015 0.013 <0.012

<0.012 <0.012 <0.012 <0.012 <0,012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.087

0.087 0.088 0.068 0.077 0.069 Savoy cabbage OD 150 Leichlingen

Germany, 2005 head

head head head head head head head -14

-11 0* 0 3 7 14 21 0.22

0.091 <0.01 0.11 0.031 <0.01 <0.01 <0.01 0.11

0.12 0.076 0.093 0.11 0.064 0.081 0.055 0.084

0.11 0.066 0.11 0.10 0.084 0.074 0.068 <0.012

<0.012 <0.012 <0.012 <0.012 <0,012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 0.434

0.341 0.172 0.333 0.261 0.178 0.185 0.153

savoy cabbage OD 150 Ennemain

N-France, 2005 head

head head head head head -14

-11 0 3 7 14 <0.01

0.013 0.013 <0.01 <0.01 <0.01 <0.012

0.015 0.024 0.031 0.026 0.027 <0.012

<0.012 0.028 0.031 0.021 0.018 <0.012

<0.012 <0.012 <0.012 <0.012 <0,012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.054

0.060 0.085 0.092 0.077 0.075

savoy cabbage OD 150 Burscheid

Germany, 2005 head

head head head head head -14

-11 0 3 7 14 0.38

0.24 0.30 <0.01 <0.01 <0.01 0.13

0.12 0.10 0.060 0.06 0.042 0.13

0.098 0.081 0.045 0.061 0.054 <0.012

<0.012 <0.012 <0.012 <0.012 <0,012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.660

0.478 0.501 0.135 0.151 0.126 Field trials – Southern Europe

red cabbage OD 100 Gavá

(Catalua) Spain, 2004 head

head head head head head 0*

0 3 7 14 23 <0.01

<0.01 <0.01 <0.01 <0.01 <0.01 0.098

0.11 0.15 0.19 0.17 0.14 0.012

0.012 0.012 0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0,012 <0.008

<0.008 <0.008 <0.008 0.008 0.008 0.140

0.152 0.192 0.232 0.212 0.182 round cabbage OD 100 Andria (BA)

Italy, 2004 head

head head head head 0*

0 3 7 14 0.01

0.07 0.01 <0.01 <0.01 0.024

0.039 0.036 0.051 0.065 0.012

0.021 0.012 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 0.066

0.150 0.078 0.093 0.107

red cabbage OD 150 Andria

Italy, 2005 head

head head head head head head head -14

-11 0* 0 3 7 14 21 0.041

<0.01 <0.01 0.030 <0.01 <0.01 <0.01 <0.01 0.036

0.025 0.031 0.047 0.046 0.058 0.062 0.071 <0.012

<0.012 <0.012 <0.012 <0.012 <0,012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0,012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 0.109

0.067 0.073 0.109 0.088 0.100 0.104 0.113

### - 118 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / fomulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330

round cabbage OD 150 Gava

Spain, 2005 head

head head head head head -16

-13 0 2 7 14 0.010

<0.01 <0.01 <0.01 <0.01 <0.01 0.019

0.022 0.032 0.029 0.032 0.034 0.020

0.018 0.017 0.017 0.014 0.018 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.069

0.070 0.079 0.076 0.076 0.082



### Where appropriate the residues from the trials perf ormed in 2005 were taken for MRL calculation, which were in correspondence with the intended GAP. Hence , the number of application did not have much influence on the resulting residues; the results of the residue trials carried out with 3 applications were taking into account for MRL calculation too. For the calculation of the MRL proposal, both of th e prescribed methods I and II have been used for spirotetramat in head cabbage (based on data obtain ed from trials from Northern and Southern Europe):

MRL-calculation based on data obtained from the Nor thern Region: Individual data points for head cabbage are: 0.067, 0.077, 0.091, 0.092, 0.097, 0.104, 0.134, 0. 151, 0.186, 0.261 mg/kg Mean residue: 0.126 mg/kg; standard deviation: 0.06 0 mg/kg STMR: 0.101 mg/kg Highest residue: 0.261 mg/kg Method I: R max 

### = 0.300 mg/kg Method II: R ber 

### = 0.320 mg/kg Based on the data available for head cabbage in nor thern Europe, a MRL of 0.5 mg/kg can be proposed.

MRL-calculation based on data obtained from the Sou thern Region: Individual data points for head cabbage are: 0.082, 0.107, 0.113, 0.232 mg/kg Mean residue: 0.134 mg/kg; standard deviation: 0.06 7 mg/kg STMR: 0.110 mg/kg Highest residue: 0.232 mg/kg Method I: R max 

### = 0.478 mg/kg Method II: R ber 

### = 0.405 mg/kg Based on the data available for head cabbage in sou thern Europe, a MRL of 0.5 mg/kg can be proposed.

Conclusion: All residue trials concerning the residue behaviour of spirotetramat in head cabbage were carried out with three applications per season. In the trials from 2 005 the first sampling was made directly after the 2 nd 

### application and three days after the 2 nd 

### application, therewith to applied GAP (2 applicati ons, spray interval 14 days) was covered by these trials. The compariso n of the specimens taken after the 2 nd 

### application and the samples 3 days after the 3 rd 

### application showed comparable results; therefore t he results of the 3 rd 

### application were taken for MRL calculation. Based o n the available trials on cauliflower and broccoli a MRL of 0.5 mg/kg for head cabbage can be proposed. Comments (RMS): No comments.

B.7.6.8.3 Leafy brassica

Spirotetramat is applied for control of aphids in l eafy brassica. The critical European GAPs for the u ses of spirotetramat in leafy brassica in northern and sou thern Europe are summarised in Table B.7.6.8.3-1.

### - 119 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.6.8.3-1: GAP for residue situation in le afy brassica

North or South of EU Indoor or

outdoor Number of

applications Mode of

application Growth stage at

last application Application rate expressed

under the relevant unit PHI (d) EU-N F 3 Spray BBCH 79 0.072 g a.s./ha 3 EU-S F 3 Spray BBCH 79 0.072 g a.s./ha 3



### Reference: Determination of the residues of BYI08330 in/on cur ly kale after spraying of BYI08330 (100 OD) in the field in United Kingdom an d Germany Author(s), year: Freitag T.; Eberhardt R.; 2006 Report/Doc. number: RA-2040/04, including trials no . R 2004 0164/7, R 2004 0165/5 M-263745-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the residues of BYI08330 in/on cur ly kale after spraying of BYI08330 (150 OD) in the field in Germany Author(s), year: Ballesteros C.; Gateaud L.; 2006 Report/Doc. number: RA-2064/05, including trials no . R 2005 0367/9, R 2005 0368/7 M-272573-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the residues of BYI08330 in/on Chi nese kale after spraying of BYI08330 (100 OD) in the field in Southern Franc e and Spain Author(s), year: Freitag T.; Eberhardt R.; 2006 Report/Doc. number: RA-2041/04, including trials no . R 2004 0166/3, R 2004 0167/1 M-264301-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the residues of BYI08330 in/on Chi nese cabbage after spraying of BYI08330 (150 OD) in the field in Spain and Italy Author(s), year: Ballesteros C.; Gateaud L.; 2006 Report/Doc. number: RA-2136/05, including trials no . R 2005 0709/7, R 2005 0710/0 M-273243-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

### - 120 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Experimental design: The magnitude of residues of spirotetramat and its metabolites in leafy brassica was determined in nor thern (4 trials on curly kale) and southern Europe (2 tri als on Chinese kale and 2 trials on Chinese cabbage ). The supervised residue trials were performed with o il based dispersion concentrate containing 100 and 150 g a.s./L respectively and were carried out in Germa ny, United Kingdom, southern France, Italy and Spai n in 2004 and 2005. In deviation to the intended GAP, th e residue trials from 2004 were conducted with a sp ray interval of 7 days. According to the critical Europ ean GAP residue data from day 3 after 3 application s were evaluated. If the total residue at later intervals exceeded the residue at day 3, residues at later in tervals were evaluated to cover the worst case. An overview on the supervised residue trials conduc ted with different formulations of spirotetramat is given in Table B.7.6.8.3-2.

Table B.7.6.8.3-2: Overview on European residue tri als with BYI08330 in leafy brassica

Location Formulation No. of trials Year Use rate

(g as/ha) Water volume No of appl. Spray interval

(days)

Field N-EU OD 100 2 2004 72 500 3 6-7 Field N-EU OD 150 2 2005 72 500-600 3 14 Field S-EU OD 100 2 2004 72-76 600-633 3 6-8 Field S-EU OD 150 2 2005 66-72 552-1500 3 14



### In 2004, samples were taken directly before and aft er the last application, 2-4, 7, 13-14 and 21 days after the last application. In 2005 the first sampling was do ne directly after the second application and 3 days later, before and after the third application and 2-3, 7, 14 and 21 days after the last application. The last application was carried out at growth stag e BBCH 43 – 78. All samples were stored deep frozen within 24 hours after sampling. The time intervals between date of deep-freezing and the last extraction ranged from 1 06 to 232 days. Analytical method used in all studies: Residues of spirotetramat and its metabolites BYI 0 8330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and BYI 08330-enol-Glc in kale and Chinese cabbage were determined by HPLC-ESI-MS/MS according to method 00857. The limit of quantification (LOQ, defined as the lowest validated fortificatio n level) was 0.01 mg/kg for spirotetramat, 0.012 mg/kg for its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and 0.008 mg/kg for BYI 08330-enol-Glc in/o n leafy brassica (all metabolites were calculated a s spirotetramat). The mean procedural recoveries at the fortification levels of 0.01 to 10.0 mg/kg for spirotetramat and its four metabolites ranged between 70 and 110 % and RSD was <20%; these results indicate that the methods used were suitable for this analysis. Findings: A detailed summary of the residue results is given in Appendix I q. The total residues of spirotetramat in leafy brassi ca (curly kale) grown in northern Europe (4 trials) ranged between 0.240 and 0.765 mg/kg. In leafy brassica (C hinese kale and Chinese cabbage) from 4 field trial s in southern Europe a total residue of 0.212 to 0.631 m g/kg could be determined. In all residue trials the number of applications and the application rates were perf ormed according to the European GAP. In the residue trials from 2004, the application interval was 7 da ys. There was no significant difference in the resi dues neither from the different spray intervals nor the different varieties nor growing areas. An overview on the results of the residue data is s ummarized in the table below. The residue values us ed for evaluation are marked with bold numbers. The total residue of spirotetramat is mainly compos ed of spirotetramat, the -enol and the -ketohydroxy metabolite. BYI08330-monohydroxy and enol-glucoside were not found or in traces, only

### - 121 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.6.8.3-3: Overview of European residue da ta for spirotetramat and its metabolites in leafy brassica used 3 times with application rates of 0.0 72 kg a.s./ha (residues are calculated as spirotetramat equivalent):

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 Field trials – Northern Europe curly Kale / 100 OD Cambridge

United Kingdom, 2004 leaf, n.

leaf, n. leaf, n. leaf, n. leaf, n. 0*

0 3 8 15 0.40

1.2 0.15 0.20 0.07 0.33

0.42 0.22 0.29 0.28 0.12

0.24 0.081 0.11 0.080 <0.012

<0.012 <0.012 <0.012 <0.012 0.008

0.008 0.008 0.008 0.012 0.870

1.880 0.471 0.620 0.454 curly Kale / 100 OD Monheim

Germany, 2004 leaf, n.

leaf, n. leaf, n. leaf, n. leaf, n. leaf, n. -1

0 3 7 14 20 0.08

1.0 0.50 0.07 0.05 0.03 0.070

0.23 0.12 0.053 0.050 0.041 0.094

0.18 0.12 0.064 0.048 0.037 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.012

0.014 0.013 0.015 0.020 0.018 0.268

1.436 0.765 0.214 0.180 0.138 curly Kale / 150 OD Monheim

Germany, 2005 leaf, n.

leaf, n. leaf, n. leaf, n. leaf, n. leaf, n. leaf, n. leaf, n. -14

-11 0* 0 3 7 14 21 1.2

0.90 0.0450 0.87 0.086 0.046 0.029 0.010 0.15

0.079 0.059 0.21 0.092 0.061 0.062 0.038 0.055

0.072 0.019 0.053 0.042 0.033 0.021 0.014 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 0.010 <0.008 1.425

1.071 0.143 1.153 0.240 0.160 0.134 0.082 curly Kale / 150 OD Burscheid

Germany, 2005 leaf, n.

leaf, n. leaf, n. leaf, n. leaf, n. leaf, n. -14

-11 0 3 7 14 1.1

0.91 1.1 0.029 0.020 0.019 0.18

0.18 0.28 0.16 0.21 0.12 0.051

0.072 0.075 0.035 0.051 0.022 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 1.351

1.182 1.475 0.244 0.301 0.181 Field trials – Southern Europe

Chinese kale / 100 OD Ouzilly

France, 2004 leaf, n.

leaf, n. leaf, n. leaf, n. 0

3 7 14 0.38

0.11 0.01 <0.01 0.37

0.28 0.19 0.15 0.11

0.12 0.056 0.046 <0.012

<0.012 <0.012 <0.012 0.029

0.034 0.037 0.039 0.901

0.556 0.305 0.257 Chinese kale / 100 OD Gava

Spain, 2004 leaf, n.

leaf, n. leaf, n

. leaf, n. leaf, n. leaf, n. 0*

0 4 7 14 20 0.10

0.47 0.08 0.07 <0.01 <0.01 0.28

0.50 0.38 0.31 0.38 0.25 0.099

0.18 0.12 0.11 0.16 0.11 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.043

0.054 0.039 0.043 0.028 0.030 0.534

1.216 0.631 0.545 0.590 0.412 Chinese cabbage / 150 OD Gava

Spain, 2005 head

head head head head head head -14

-12 0 2 7 14 21 0.94

0.28 <0.01 <0.01 <0.01 <0.01< 0.01 0.72

0.49 0.12 0.19 0.16 0.082 0.060 0.13

0.15 0.047 0.069 0.12 0.068 0.055 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 1.810

0.940 0.197 0.289 0.310 0.180 0.145 Chinese cabbage / 150 OD Andria

Italy, 2005 head

head head head head head head head -14

-11 0* 0 3 7 14 21 0.048

<0.01 <0.01 0.020 <0.01 <0.01 <0.01 <0.01 0.11

0.16 0.11 0.11 0.13 0.15 0.13 0.13 0.033

0.028 0.021 0.029 0.026 0.032 0.026 0.035 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 0.211

0.218 0.161 0.179 0.186 0.212 0.186 0.195 leaf, n. = leaf, normal

### - 122 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Leafy brassica is classified as minor crops in nort hern and southern Europe. For extrapolation to the whole group of leafy brassica, a minimum of 4 trials on k ale are required. For the calculation of the MRL proposal, both of th e prescribed methods I and II have been used for spirotetramat in leafy brassica (based on data obta ined from trials from northern and southern Europe) :

MRL-calculation based on data obtained from the Nor thern Region: Individual data points for curly kale are: 0.240, 0.301, 0.620, 0.765 mg/kg Mean residue: 0.482 mg/kg; standard deviation: 0.25 2 mg/kg STMR: 0.461 mg/kg Highest residue: 0.765 mg/kg Method I: R max 

### = 1.778 mg/kg Method II: R ber 

### = 1.458 mg/kg Based on the data available for leafy brassica in n orthern Europe, a MRL of 2 mg/kg can be proposed.

MRL-calculation based on data obtained from the Sou thern Region: Individual data points for Chinese kale are: 0.556, 0.631 mg/kg Individual data points for Chinese cabbage are: 0.212, 0.310 mg/kg Mean residue: 0.427 mg/kg; standard deviation: 0.19 8 mg/kg STMR: 0.433 mg/kg Highest residue: 0.631 mg/kg Method I: R max 

### = 1.448 mg/kg Method II: R ber 

### = 1.225 mg/kg Based on the data available for leafy brassica in s outhern Europe, a MRL of 2 mg/kg can be proposed.

Conclusion: In 2004 and 2005, altogether 8 residue trials in No rthern and Southern Europe were carried out. Apart from the spray interval, all trials were carried out acc ording the intended use parameters and were perform ed as residue decline studies. There was no difference in residues of total spirotetramat in leafy brassica grown in northern or southern Europe. Based on the submitted supervised residue trials a MRL of 2 mg/kg can be proposed. Comments (RMS): No comments.

B.7.6.8.4 Kohlrabi

Spirotetramat is applied for the use in kohlrabi in northern Europe against aphids. The critical Europ ean GAPs are summarised in table B.7.6.8.4-1.

Table B.7.6.8.4-1: GAP for residue situation in k ohlrabi

North or South of EU Indoor or

outdoor Number of

applications spray

interval Mode of

application Growth stage at

last application Application rate PHI

(d) EU-N F 2 14 days Spray BBCH 79 72 g a.s./ha 3

### - 123 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Reference: Determination of the Residues of BYI08330 in/on Koh lrabi after Spraying of BYI08330 (100 OD) in the Field in Germany and the N etherlands Author(s), year: Freitag T.; Eberhardt R.; 2006 Report/Doc. number: RA-2043/04, including trials no . R 2004 0169/8, R 2004 0170/1 M-265036-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the Residues of BYI08330 in/on Koh lrabi after Spraying of BYI08330 (150 OD) in the Field in Germany Author(s), year: Freitag T.; Eberhardt R.; 2006 Report/Doc. number: RA-2065/05, including trials no . R 2005 0373/3, R 2005 0374/1 M-272128-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Experimental design: The magnitude of residues of spirotetramat and its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-mono-hydroxy and BYI 08330-enol-Glc in/on koh lrabi harvested following the treatment with spirotetramat formulations (100 OD, 150 OD) was det ermined in northern Europe (Germany and The Netherlands) in 2004 and 2005. In northern Europe 4 trials on kohlrabi were perfor med using different formulations of spirotetramat. An overview on the supervised residue trials conducted with different formulations of spirotetramat is gi ven in table B.7.6.8.4-2.

Table B.7.6.8.4-2: Overview on European residue tri als with spirotetramat in kohlrabi

Location Formulation No. of trials Year Use rate

(g as/ha) Water volume No of appl. Spray interval

(days) Field N-EU OD 100 2 2004 72 400, 600 L/ha 3 7-8 Field N-EU OD 150 2 2005 72 600, 1000 L/ha 3 14-15



### In 2004, the residue trials were carried out with 3 spray applications of spirotetramat and a spray in terval of 7 days. Samples of leaves and the corm were taken bef ore and after the last application, 0, 3, 7, 14 and 21 days after the last application. The notifier state d that due to new results from biological trials th e critical GAP changed: The number of applications was changed fro m 3 to 2 and the spray interval from 7 days to 14 d ays. Therefore the residue trials from 2005 were perform ed with 3 applications and a spray interval of 14 d ays. Samples were taken directly after the second applic ation, and 3 days later (to cover the use pattern w ith two applications), before and after the third applicati on, 3, 7, 14 and 21 days after the last application

. The last application was carried out at growth stag e BBCH 17 – 47. All samples were stored deep frozen within 24 hours after sampling. The time intervals between date of deep-freezing and the last extraction ranged from 1 73 to 463 days. Analytical method used in all studies: Residues of spirotetramat and its metabolites BYI 0 8330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and BYI 08330-enol-Glc were determined by H PLC-ESI-MS/MS according to method 00857.

### - 124 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

The limit of quantification (LOQ, defined as the lowest validated fortificatio n level) was 0.01 mg/kg for spirotetramat, 0.012 mg/kg for its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and 0.008 mg/kg for BYI 08330-enol-Glc in/o n kohlrabi leaves and corm (all metabolites were calculated as spirotetramat equivalent). The mean procedural recoveries at the fortification levels of 0.01 to 10.0 mg/kg for spirotetramat and its four metabolites ranged between 70 and 110 % and RSD was <20%; these results indicate that the methods used were suitable for this analysis. Findings: A detailed summary of the residue results is given in Appendix I r. All residue trials for the residue behaviour of spi rotetramat on kohlrabi were carried out with 3 appl ications per seasons. The number of applications and differe nt spray intervals in the submitted trials carried out in 2004 are not fully in accordance with the intended use for kohlrabi. In the residue trials performed i n 2005, the first specimens were taken directly after the 2 nd 

### application and 3 days later, therefore it was pos sible to compare the residues after three and two applicatio ns. Neither the number of applications nor the time int erval between the applications seemed to have an influence on the resulting residues. Residues of to tal spirotetramat in kohlrabi after 3 applications ranged between 0.152 and 0.670 mg/kg whereas after 2 appli cations residues of 0.204 and 0.267 mg/kg were detected. An overview on the results of the residue data is summarized in the table below. The residue values used for evaluation are marked with bold num bers. The total residue of spirotetramat in kohlrabi corm is mainly composed of the -enol and the ketohydrox y metabolites. The parent compound and the enol-gluco side were present at lower amounts. BYI08330- monohydroxy was not detected or in traces, only.

Table B.7.6.8.2.2-3: Overview of northern European residue data for spirotetramat and its metabolites in kohlrabi used 3 times with application rates of 0.072 kg a.s./ha:

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330

kohlrabi / OD 100 WerlWestönnen Germany, 2004 corm

leaf, n.

corm leaf, n.

corm leaf, n.

corm leaf, n.

corm leaf, n.

corm leaf, n. 0*

0* 0 0 3 3 7 7 14 14 21 21 0.01

0.04 0.03 1.2 0.01 0.66 0.01 0.06 <0.01 <0.01 <0.01 <0.01 0.42

0.41 0.55 2.1 0.52 1.2 0.51 0.73 0.33 0.10 0.13 0.023 0.064

0.11 0.11 0.48 0.12 0.29 0.083 0.14 0.020 0.032 0.012 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

0.021 0.008 0.023 0.008 0.027 <0.008 0.028 <0.008 0.017 <0.008 0.014 0.514

0.593 0.710 3.815 0.670 2.189 0.623 0.970 0.380 0.171 0.172 0.071 kohlrabi / OD 100 ZwaagdijkOost Netherlands , 2004 corm

leaf, n.

corm leaf, n.

corm leaf, n.

corm leaf, n.

corm leaf, n.

corm leaf, n. 0*

0* 0 0 3 3 7 7 14 14 21 21 <0.01

0.08 0.01 1.5 0.01 0.91 <0.01 0.49 <0.01 0.05 <0.01 0.01 0.37

0.10 0.42 0.62 0.42 0.35 0.49 0.16 0.28 0.041 0.20 0.041 0.032

0.038 0.038 0.21 0.033 0.097 0.034 0.059 0.018 0.012 0.012 0.012 <0.012

<0.012 <0.012< 0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012< 0.012 <0.008

0.033 <0.008 0.042 <0.008 0.042 0.008 0.056 0.008 0.067 <0.008 0.061 0.432

0.263 0.488 2.384 0.483 1.411 0.554 0.777 0.328 0.182 0.242 0.136

### - 125 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330

kohlrabi / OD 150 LangenfeldReusrath Germany, 2005 corm

leaf, n.

corm leaf, n.

corm leaf, n.

corm leaf, n.

corm leaf, n.

corm leaf, n.

corm leaf, n.

corm leaf, n. -14

-14 -11 -11 0* 0* 0 0 3 3 7 7 14 14 21 21 0.01

0.57 0.01 0.12 0.01 1.1 0.01 1.3 0.01 0.08 0.01 0.10 <0.01 0.02 <0.01 0.01 0.096

0.87 0.22 0.18 0.15 0.42 0.13 0.41 0.19 0.14 0.15 0.032 0.094 0.012 0.045 0.012 0.013

0.28 0.017 0.062 0.013 0.11 0.013 0.12 0.012 0.044 0.012 <0.012 0.012 <0.012 0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

0.022 <0.008 0.025 <0.008 0.022 <0.008 0.022 <0.008 0.038 <0.008 0.040 <0.008 0.032 <0.008 0.029 0.139

1.754 0.267 0.399 0.193 1.664 0.173 1.864 0.232 0.314 0.192 0.196 0.136 0.088 0.087 0.075 kohlrabi / OD 150 Burscheid

Germany, 2005 corm

leaf, n.

corm leaf, n.

corm leaf, n.

corm leaf, n.

corm leaf, n.

corm leaf, n.

corm leaf, n. -14

-14 -11 -11 0* 0* 0 0 3 3 7 7 14 14 0.03

1.3 0.01 0.38 0.02 0.77 0.01 0.03 <0.01 0.01 <0.01 0.01 <0.01 <0.01 0.18

0.38 0.16 0.17 0.13 0.24 0.11 0.027 0.11 0.074 0.088 0.045 0.068 0.023 0.015

0.044 0.014 0.025 0.012 0.034 0.012 0.012 0.012 0.014 0.012 0.012 0.012 0.012 <0.012

<0.012 <0.012< 0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.008

0.038 0.008 0.044 0.008 0.054 <0.008 0.048 <0.008 0.062 <0.008 0.057 <0.008 0.052 0.245

1.774 0.204 0.631 0.182 1.11 0.152 0.129 0.152 0.172 0.13 0.136 0.110 0.109 leaf, n. leaf, normal



### Hence, the number of application did not have much influence on the resulting residues the results of the residue trials carried out with 3 applications were taking into account for MRL calculation too. For the calculation of the MRL proposal, both of th e prescribed methods I and II have been used for spirotetramat in kohlrabi (based on data obtained f rom trials from Northern Europe):

MRL-calculation based on data obtained from the nor thern region: Individual data points for kohlrabi are: 0.152, 0.232, 0.554, 0.670 mg/kg Mean residue: 0.402 mg/kg; standard deviation: 0.24 9 STMR: 0.393 mg/kg Highest residue: 0.670 mg/kg Method I: R max 

### = 1.684 mg/kg Method II: R ber 

### = 1.282 mg/kg Based on the data available for kohlrabi in norther n Europe, a MRL of 2 mg/kg can be proposed. Conclusion: Kohlrabi is applied for the use of spirotetramat in northern Europe. 4 supervised residue trials were submitted to support this use. All trials were carried out wi th 3 applications. In 2005, the first sampling was made directly after the second application and the next samples were taken three days after the second application, to cover the GAPs with two and three a pplications (according the intended use). The resul ts from these trials are well corresponding to those from t he other trials carried out with 3 applications. Th erefore the

### - 126 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

trials conducted with 3 applications were considere d in the MRL-calculation. The residues of spirotetr amat and its metabolites on kohlrabi ranged between 0.15 2 – 0.670 mg/kg. The data is sufficient to propose an EU MRL (based on N-EU data) and a MRL of 2 mg/kg can be proposed. Comments (RMS): No comments.

B.7.6.9 Green bean (fresh, with pods)

Spirotetramat is applied for control of aphids, whi te flies and mites on bean and pea plants. The crit ical European GAP for the uses of spirotetramat on green beans in glasshouse is summarised in table B.7.6.9 -1.

Table B.7.6.9-1: GAP for residue situation in gree n beans

North or South of EU Indoor or

outdoor Number of

applications spray

interval Mode of

application Growth stage at

last application Application rate PHI

(d) EU-N/S G 4 7 days Spray BBCH 87 0.072 g a.s. / ha and m leafy surface* 14



### Reference: Determination of the residues of BYI08330 in/on cli mbing French bean after spraying of BYI08330 (100 OD) in the greenhouse in Italy, Germany and Southern France Author(s), year: Schöning R.; Wolters A.; 2006 Report/Doc. number: RA-2042/04, including trials no . R 2004 0172/8, R 2004 0173/6, R 2004 0174/4, R 2004 0175/2, R 2004 0176/0, R 2004 0177/9, R 2004 0 178/7, R 2004 0179/5 M-263646-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Experimental design: The magnitude of residues of spirotetramat and its metabolites in green beans was determined in northe rn and southern Europe for the protected use in glassh ouses. In 2004, the supervised residue trials carried out in Germany, southern France, Italy and Spain were performed on climbing French beans with oil based d ispersion concentrate containing 100 g a.s./L . The trials were conducted in accordance to the critical European GAP. The application of 72 g as/ha and m plant height (plants height: 1.2 m - 2 m) resulted in app lication rates of 86.4 - 144 g a.s./ha. An overview on the supervised residue trials conduc ted with different formulations of spirotetramat is given in Table B.7.6.9-2.

Table B.7.6.9-2: Overview on European residue tria ls with spirotetramat in green beans

Location Formulation No. of trials Year Use rate

(g as/ha)* Water volume* No of appl. Spray interval

(days)

Field N/S-EU OD 100 8 2004 72 500 4 14-21 * the application rate is adapted to the height of the leafy surface



### Samples were taken directly before and after the la st application, 7, 10, 14 and 21 days after the las t application. The last application was carried out at growth stag e BBCH 71 – 79. All samples were stored deep frozen within 24 hours after sampling. The time intervals between date of deep-freezing and the last extraction ranged from 1 63 to 268 days.

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Analytical method used in all studies: Residues of spirotetramat and its metabolites BYI 0 8330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and BYI 08330-enol-Glc in climbing French b eans with pods were determined by HPLC-ESI-MS/MS according to method 00857. The limit of quantification (LOQ, defined as the lowest validated fortificatio n level) was 0.01 mg/kg for spirotetramat, 0.012 mg/kg for its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and 0.008 mg/kg for BYI 08330-enol-Glc in/o n beans with pods (all metabolites were calculated as spirotetramat equivalent). The mean procedural recoveries at the fortification levels of 0.01 to 10.0 mg/kg for spirotetramat and its four metabolites ranged between 70 and 110 % and RSD was <20%; these results indicate that the methods used were suitable for this analysis. Findings: A detailed summary of the residue results is given in Appendix I s. The total residues of spirotetramat in green beans with pods grown in European glasshouses ranged between 0.082 and 0.624 mg/kg. An overview on the results of the residue data is s ummarized in the table below. The residue values us ed for evaluation are marked with bold numbers.

Table B.7.6.9-3: Overview of European residue data for spirotetramat and its metabolites in green beans used 4 times with application rates of 0.072 kg a.s./ha and m leafy surface; formulation OD100:

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 Field trials – glasshouse climbing French bean Palidoro

Fiumicino Italy, 2004 bean w.p

bean w.p bean w.p. bean w.p. bean w.p. bean w.p. 0*

0 7 10 14 21 0.03

0.24 0.13 0.06 0.06 0.04 0.17

0.26 0.25 0.11 0.12 0.063 0.19

0.22 0.20 0.12 0.081 0.042 <0.012

0.012 0.012 0.012 0.012 0.012 0.024

0.030 0.038 0.025 0.030 0.023 0.426

0.762 0.630 0.327 0.303 0.180 climbing French bean Manfredonia

Italy, 2004 bean w.p

bean w.p bean w.p. bean w.p. bean w.p. bean w.p. 0*

0 7 10 14 21 0.19

0.42 0.52 0.28 0.01 0.01 0.25

0.46 0.34 0.25 0.066 0.036 0.077

0.12 0.089 0.076 0.020 0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.021

0.025 0.035 0.029 0.008 0.008 0.550

1.037 0.996 0.647 0.116 0.0780 climbing French bean Langenfeld

Germany, 2004 bean w.p

bean w.p bean w.p. bean w.p. bean w.p. bean w.p. 0*

0 7 10 14 21 0.16

0.20 0.15 0.04 0.13 0.03 0.23

0.22 0.27 0.23 0.29 0.19 0.11

0.13 0.12 0.099 0.099 0.055 <0.012

<0.012 0.012 0.012 0.012 0.012 0.018

0.018 0.026 0.021 0.035 0.032 0.530

0.580 0.578 0.402 0.566 0.319 climbing French bean Rognonas

S-France, 2004 bean w.p

bean w.p bean w.p. bean w.p. bean w.p. bean w.p. 0*

0 7 10 14 21 0.10

0.28 0.22 0.35 0.15 0.04 0.088

0.15 0.24 0.28 0.26 0.19 0.16

0.21 0.17 0.10 0.099 0.080 0.012

0.012 0.012 0.012 0.012 0.012 0.024

0.025 0.033 0.040 0.043 0.054 0.384

0.677 0.675 0.782 0.564 0.376 climbing French bean FurbaraCerveteri Italy, 2004 bean w.p

bean w.p bean w.p. bean w.p. bean w.p. bean w.p. 0*

0 7 10 14 21 0.01

0.04 0.01 0.01 0.01 <0.01 0.041

0.054 0.049 0.031 0.015 <0.012 0.10

0.10 0.11 0.070 0.037 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.009

0.010 0.014 0.012 0.008 <0.008 0.172

0.216 0.195 0.135 0.082 0.054

### - 128 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 climbing French bean Molfetta

Italy, 2004 bean w.p

bean w.p bean w.p. bean w.p. bean w.p. bean w.p. 0*

0 7 10 14 21 0.01

0.08 0.02 0.01 0.01 <0.01 0.037

0.082 0.068 0.046 0.090 0.026 0.084

0.20 0.14 0.075 0.084 0.023 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 0.009

0.009 0.012 0.009 0.012 0.008 0.152

0.383 0.252 0.152 0.208 0.079 climbing French bean Noves

S-France, 2004 bean w.p

bean w.p bean w.p. bean w.p. bean w.p. bean w.p. 0*

0 7 10 14 21 0.06

0.13 0.08 0.13 0.11 0.13 0.10

0.13 0.22 0.26 0.27 0.29 0.14

0.17 0.16 0.11 0.12 0.12 0.012

0.012 0.012 0.012 0.012 0.017 0.020

0.020 0.027 0.031 0.043 0.067 0.332

0.462 0.499 0.543 0.555 0.624 climbing French bean Langenfeld

Germany, 2004 bean w.p

bean w.p bean w.p. bean w.p. bean w.p. bean w.p. 0*

0 7 10 14 21 0.02

0.09 0.06 0.07 0.04 0.02 0.23

0.26 0.40 0.36 0.23 0.15 0.16

0.14 0.11 0.13 0.098 0.061 0.012

<0.012 0.012 0.012 <0.012 <0.012 0.012

0.012 0.023 0.022 0.021 0.015 0.434

0.514 0.605 0.594 0.401 0.258

* Before the last treatment ** Residues of each analyte calculated as spirotetr amat (BYI 08330) bean w.p. bean with pod



### The total residue of spirotetramat in green beans i s mainly composed of spirotetramat, the enol and th e ketohydroxy metabolites. BYI 08330 monohydroxy and enol-glucoside were not detected or in traces, only

. For the calculation of the MRL proposal, both of th e prescribed methods I and II have been used for spirotetramat in green beans (based on data obtaine d from glasshouse trials from northern and southern Europe):

MRL-calculation based on data obtained from the gla sshouse trials: Individual data points for green beans are: 0.082, 0.116, 0.208, 0.303, 0.401, 0.564, 0.566, 0. 624 mg/kg Mean residue: 0.358 mg/kg; standard deviation: 0.21 3 mg/kg STMR: 0.352 mg/kg Highest residue: 0.624 mg/kg Method I: R max 

### = 1.038 mg/kg Method II: R ber 

### = 1.131 mg/kg Based on the data available for green beans cultiva ted in glasshouses, a MRL of 2 mg/kg can be proposed. Conclusion: In 2004, 8 supervised residue glasshouse trials in Northern and Southern Europe were carried out. All trials were conducted according the intended GAP. Based on the submitted supervised residue trials a MRL of 2 mg/kg can be proposed. Comments (RMS): No comments.

B.7.6.10 Hops

Spirotetramat is applied for control of aphids, sca les and mites in hops. The critical European GAP fo r the uses of spirotetramat on hop from northern Europe i s summarised in table B.7.6.10-1.

### - 129 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.6.10-1: GAP for residue situation in ho ps North or South of EU Indoor or

outdoor Number of

applications spray

interval Mode of

application Growth stage at

last application Application rate PHI

(d) EU-N F 1 n.a. Spray BBCH 75 150 g a.s./ha 14 n.a. not applicable



### Reference: Determination of the Residues of BYI08330 in/on Hop after Spraying of BYI08330 (100 OD) in the Field in Northern France a nd Germany Author(s), year: Schöning R.; Helfrich P.; 2006 Report/Doc. number: RA-2036/04, including trials no . R 2004 0148/5, R 2004 0149/3, R 2004 0150/7, R 2004 0151/5 M-265047-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Reference: Determination of the Residues of BYI08330 in/on Hop after Spraying of BYI08330 (150 OD) in the Field in Germany and North ern France Author(s), year: Schöning R.; 2006 Report/Doc. number: RA-2108/05, including trials no . R 2005 0550/7, R 2005 0551/5, R 2005 0552/3, R 2005 0553/1 M-272100-01-1 Guideline(s): EU Council Directive 91/414/EEC Annex II, part A section 6 and Annex III, part A, section 8 residues in or on treated products, food and feed GLP: Yes Deviations: No Validity: Yes

Experimental design: The magnitude of residues of spirotetramat and its metabolites on hops was determined in northern Euro pe in 2004 and 2005. The supervised residue trials on hop, carried out in Germany and northern France wer e performed with oil based dispersion concentrates co ntaining 100 and 150 g a.s./L respectively. In 2004 , all trials were conducted with 2 applications and an ap plication rate of 175 g a.s./ha, the spray interval was 13- 15 days. Due to new result from biological trials t he GAP for the use of spirotetramat in hops was cha nged from two applications of 175 g as/ha to one applica tion of 150 g as/ha. Hence residue trials in 2005 w ere conducted according to the new critical European GA P. An overview on the supervised residue trials conduc ted with different formulations of spirotetramat is given in Table B.7.6.10-2.

Table B.7.6.10-2: Overview on European residue tri als with spirotetramat on hop

Location Formulation No. of trials Year Use rate

(g as/ha)* Water volume* No of appl. Spray interval

(days)

Field N -EU OD 100 4 2004 175 2200-2500 2 13-15 Field N -EU OD 150 4 2005 150 2000-2200 1 n.a. n.a. not applicable



### Samples of green cones were taken after the last ap plication, 7-8, 13-15, 20-22 and 28-29 days after t he last application; at the trials from 2004 in addition sa mples directly before the 2 nd 

### application were taken. Except on day 0, cones were kiln-dried until approx 10% re maining moisture directly after sampling for labora tory sample.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

The last application was carried out at growth stag e BBCH 72 – 86. All samples were stored deep frozen within 24 hours after sampling. The time intervals between date of deep-freezing and the last extraction ranged from 1 25 to 366 days. Analytical method used in all studies: Residues of spirotetramat and its metabolites BYI 0 8330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and BYI 08330-enol-Glc in green and kiln-dr ied hops cons were determined by HPLC-ESI-MS/MS according to method 00857. The limit of quantification (LOQ, defined as the lowest validated fortificatio n level) was 0.1 mg/kg for spirotetramat, 0.12 mg/kg for its metabolites BYI 0 8330-enol, BYI 08330-ketohydroxy, BYI 08330-monohydroxy and 0.08 mg/kg for BYI 08330-enol-Glc in/on green and kiln-dried cone (all metabolites were calculated as spirotetramat equivalent). The mean procedural recoveries at the fortification levels of 0.1 to 10.0 mg/kg f or spirotetramat and its four metabolites ranged between 70 and 110 % and RSD was <20%; these results indicate that the methods used were suitable for this analysis. Findings: A detailed summary of the residue results is given in Appendix I t. The supervised residue trials in 2004 were performe d with 2 applications in stead of 1 application onl y; therefore, these trials were not conducted accordin g to the intended GAP. The residue data on green co nes obtained from residue trials carried out in 2004 re sidue data are available for samples collected 14 d ays after the first application, but these specimens were not further kiln-dried. The residues of total spirotet ramat in green cones after one application ranged between 0. 54 and 0.90 mg/kg whereas after 2 applications residues between 0.60 and 1.20 mg/kg were detected. Therefore, the number of applications seemed to have no significant influence on the resulting resi dues. In 2004 the application rate of spirotetramat was 1 75 g as/ha exceeding the application rate of the cr itical European GAP by 17%. The divergence between the app lication rates is within the 25 % tolerance accordi ng to the guideline (SANCO Document 7525/VI/95 rev.7) and is regarded as acceptable. An overview on the results of the residue data is s ummarized in the table below. The residue values us ed for evaluation are marked with bold numbers.

Table B.7.6.10-3: Overview of European residue data for spirotetramat and its metabolites in green and kiln-dried cones used 1-2 times with applicatio n rates of 0.175-150 kg a.s./ha (residues are calculated as spirotetramat equivalent):

crop / No of appl./ formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 Field trials – Northern Europe hop 2 appl. OD 100 Schleithal

N-France, 2004 cone, g.

cone, g. cone, g. cone, KD cone, g. cone, KD

cone, g cone, KD 0*

0 8 8 14 14 22 22 0.40

0.58 0.11 0.24 0.17 0.63 0.10 0.52 <0.12

0.18 <0.12 0.23 <0.12 0.18 <0.12 0.15 <0.12

<0.12 <0.12 0.19 <0.12 0.30 <0.12 0.19 <0.12

<0.12 <0.12 <0.12 <0.12 <0.12 <0.12 <0.12 0.14

0.31 0.09 0.27 0.13 0.41 0.09 0.43 0.90

1.31 0.56 1.05 0.66 1.64 0.55 1.41 hop 2 appl. OD 100 Gebrontshausen Germany, 2004 cone,g.

cone, g. cone, g. cone, KD

cone, g. cone, KD

cone g. cone, KD 0*

0 7 7 14 14 22 22 0.21

1.50 0.25 1.7 0.27 0.56 0.26 0.94 <0.12

0.67 0.21 0.97 <0.12 0.25 <0.12 0.35 <0.12

0.27 0.23 1.0 0.17 0.39 0.15 0.51 <0.12

<0.12 <0.12 <0.12 <0.12 <0.12 <0.12 <0.12 0.14

0.19 0.25 1.0 0.21 0.50 0.23 0.70 0.71

2.75 1.06 4.79 0.89 1.82 0.88 2.62

### - 131 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

crop / No of appl./ formulation Location,

year portion DAT [days] BYI

08330 BYI

08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total

residues of BYI 08330 hop 2 appl. OD 100 Tettnang

Germany, 2004 cone, g.

cone g. cone, g. cone, KD

cone, g. cone, KD

cone g. cone, KD

cone, g. 0*

0 7 7 14 14 21 21 28 0.14

0.98 0.43 2.0 0.19 1.1 0.25 1.2 0.26 0.31

0.88 0.27 1.1 <0.12 0.75 0.14 0.58 0.20 <0.12

0.24 0.34 1.4 0.14 0.75 0.16 0.60 0.17 <0.12

<0.12 <0.12 <0.12 <0.12 <0.12 <0.12 <0.12 <0.12 0.21

0.39 0.38 1.6 0.26 1.30 0.30 1.2 0.46 0.90

2.61 1.54 6.22 0.83 4.02 0.97 3.70 1.21 hop 2 appl. OD 100 Obernai

N-France, 2004 cone, g.

cone g. cone, g. cone, KD

cone, g. cone, KD

cone g. cone, KD

cone, g. 0*

0 8 8 15 15 22 22 29 0.14

0.97 0.70 2.3 0.63 2.6 0.53 2.2 0.53 <0.12

0.32 <0.12 0.28 <0.12 0.32 <0.12 0.25 <0.12 <0.12

0.20 0.22 0.62 0.19 0.72 0.13 0.45 <0.12 <0.12

<0.12 <0.12 <0.12 <0.12 <0.12 <0.12 <0.12 <0.12 0.10

0.10 0.15 0.36 0.14 0.58 0.15 0.49 0.15 0.60

1.71 1.31 3.68 1.20 4.34 1.05 3.51 1.04 hop 1 appl. OD 150 Gebrotshausen Germany, 2005 cone, g.

cone, g. cone, g. cone, KD

cone, g. cone, KD 0

7 14 14 21 21 0.85

0.28 0.15 1.5 0.11 0.93 0.24

0.12 <0.12 0.19 <0.12 0.21 <0.12

<0.12 <0.12 <0.12 <0.12 <0.12 <0.12

<0.12 <0.12 <0.12 <0.12 <0.12 <0.08

0.08 0.08 0.08 0.08 0.08 1.41

0.72 0.59 2.01 0.55 1.46 hop 1 appl. OD 150 Schleithal

N-France, 2005 cone, g.

cone, g. cone, g. cone, KD

cone, g. cone, KD 0

7 13 13 20 20 0.94

0.28 0.15 0.83 0.10 0.60 0.30

0.12 0.12 0.23 0.12 0.14 <0.12

<0.12 <0.12 0.43 <0.12 0.21 <0.12

<0.12 <0.12 <0.12 <0.12 <0.12 <0.08

0.08 0.08 0.13 0.08 0.13 1.56

0.72 0.59 1.74 0.54 1.20 hop 1 appl. OD 150 Tettnang

Germany, 2005 cone, g.

cone, g. cone, KD

cone, g. cone, KD 0

14 14 21 21 0.98

0.32 1.5 0.21 1.1 0.36

0.12 0.32 0.12 0.31 <0.12

0.17 0.88 0.12 0.52 <0.12

<0.12 <0.12 <0.12 <0.12 <0.08

0.08 0.29 0.08 0.33 1.66

0.81 3.11 0.65 2.38 hop 1 appl. OD 150 Obernai

N-France, 2005 cone, g.

cone, g. cone, KD

cone, g. cone, KD 0

14 14 21 21 0.42

<0.1 0.61 <0.1 0.47 0.12

<0.12 0.12 <0.12 0.12 <0.12

<0.12 0.18 <0.12 0.13 <0.12

<0.12 <0.12 <0.12 <0.12 <0.08

<0.08 0.08 <0.08 0.08 0.86

0.54 1.11 0.54 0.92

* Before the last treatment ** Residues of each analyte calculated as spirotetr amat (BYI 08330) cone, g. cone, green cone, KD cone, kiln-dried



### The total residue in kiln-dried cones is composed o f BYI08330, the enol, ketohydroxy and enol-glucosid e metabolite. BYI08330-monohydroxy was not found.

For the calculation of the MRL proposal, both of th e prescribed methods I and II have been used for spirotetramat in hops (based on data obtained from glasshouse trials from northern Europe): MRL-calculation based on data obtained from the Nor thern Region: Individual data points for hops are: 1.11, 1.64, 1.74, 2.01, 2.62, 3.11, 4.02, 4.34 mg/k g Mean residue: 2.574 mg/kg; standard deviation: 1.16 7 mg/kg STMR: 2.315 mg/kg

### - 132 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Highest residue: 4.34 mg/kg Method I: R max 

### = 6.293 mg/kg Method II: R ber 

### = 7.585 mg/kg Based on the data available for hops from northern Europe, a MRL of 10 mg/kg can be proposed. Conclusion: In 2004, 4 supervised residue trials in Northern Eu rope were carried out. These trials were conducted with to applications and a 17 % higher application rate wit h an interval between the applications of 14 days. Hence there was no significant difference between the res ults on green cones before and 14 days after the 2 nd 

### application, the results from these trials were con sidered for MRL calculation. The residue trials con ducted in 2005 were in accordance to the intended GAP. Based on the submitted supervised residue trials a MRL of 10 mg/kg can be proposed. Comments (RMS): No comments.

B.7.6.11 Overall conclusion

Residue data from field trials on uses of spirotetr amat in citrus, lettuce, fruiting vegetables, brass ica vegetables and hops conducted in various locations all over Europe are reported and evaluated in order to accelerate the fixing of MRLs with respect to Regul ation 396/2005/EU. Spirotetramat is applied as a spray solution to the different crops. Different formulations of spirote tramat were used: In 2004, residue trials were conducted w ith the OD 100 formulation of BYI08330. Due to a mi nor change of the final formulation from OD 100 to OD 1 50, residue trials in 2005 were conducted with the OD 150 formulation of BYI08330. The composition of bot h formulations is similar; but the amount of the ac tive substance is 100 g as/L in the OD 100 formulation a nd 150 g as/L in the OD 150 formulation. Applied at identical use rates for the active substance, both formulations are considered to be comparable with r espect to residues. Results from additional residue trials in lettuce a nd pepper are reported, which were conducted using the SC 240 formulation of BYI08330 with the addition of 0. 2 % RME (rape methyl ester) to the spray solution. Moreover, 2 trials in pepper were conducted with th e SC 048 formulation of BYI08330. The results of th ese trials are reported to give a complete picture of t he BYI08330 residue behaviour.

Analysis of residue samples was conducted according to method 0087. The single analytes (spirotetramat and its metabolites BYI08330-enol, -ketohydroxy, -m onohydroxy and -enol-glucoside) are determined by HPLC-MS/MS. The results are expressed as parent equ ivalents. The total residue of spirotetramat is calculated by summing up the values determined for the individual analytes expressed as parent equival ent. Expressed as parent equivalents the LOQ is 0.01 mg/ kg for spirotetramat, 0.012 mg/kg for BYI08330-enol , - ketohydroxy and –monohydroxy and 0.08 mg/kg for BYI 08330-enol-glucoside. For hop cones the respective LOQs are by a factor of 10 higher. The LOQ for the calculated total residue of BYI08330 is quoted at 0 .054 mg/kg (hops 0.54 mg/kg). For each trial residues at the envisaged PHI of the critical GAP were evaluated. If, however, the tota l residue of spirotetramat at later intervals exceeded the to tal residue at the PHI, the higher values were eval uated to cover the worst case residue. The residue data of each trial used for the evaluat ion are reported in the tables of Annex I at the en d of the residue section.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

B.7.6.12 Stability of residues prior to analysis

B.7.6.12.1 Storage stability in plant commodities

Reference: Storage Stability of BYI 08330 and its Metabolites BYI08330-enol, BYI08330- ketohydroxy, BYI08330-mono-hydroxy and BYI08330-eno l-glucoside in/on Tomato (Fruit), Tomato (Paste), Potato (Tuber), Let tuce (Head), Climbing French Bean (Bean With Pod), and Almond (Nutmeat) f or 24 Months. Author(s), year: Schöning, R., Wolters, A. (2007) Report/Doc. number: Report No.: MR-07/268, Edition Number: M-289421-01-2 Guideline(s): PMRA Directive 98-02; DACO 7.3/EPA OP PTS 860.1380 GLP: Yes. Deviations: No. Validity: Yes.

Reference: Storage Stability of BYI 08330 and its Metabolites BYI08330-enol, BYI08330- ketohydroxy, BYI08330-mono-hydroxy and BYI08330-eno l-glucoside in/on Orange (juice) and Prunes (Fruit) for 5 Months. Author(s), year: Schöning, R., Wolters, A. (2006) Report/Doc. number: Report No.: MR-06/076, Edition Number: M-276529-02-1 Guideline(s): PMRA Directive 98-02; DACO 7.3/EPA OP PTS 860.1380 GLP: Yes. Deviations: No. Validity: Yes.

Material and methods:

Samples of tomato (fruit and paste), potato (tuber) , lettuce (head), climbing French bean (bean with p od) and almond (nutmeat) were spiked separately with 0.2 pp m of each spirotetramat (BYI 08330), BYI 08330-enol

, BYI 08330-ketohydroxy, BYI 08330-mono-hydroxy, BYI 08330-enol-glucoside and stored at -18oC for approximately 30, 60, 90, 180, 370, 540, and 718 da ys. Samples spiked with BYI08330-enol were also analyzed for all analytes, with the exception of sp irotetramat, and the total residues were expressed as BYI08330-enol equivalents. Samples that were spiked with BYI08330-ketohydroxy or BYI08330-monohydroxy or BYI08330-enol-Glc were analyzed and repo rted individually. Samples were analyzed by highperformance liquid chromatography with tandem mass spectrometry (HPLC-MS/MS) method 00857 using internal standards. Adequate method validation data were provided.

A second study was performed to examine the effects of frozen storage on spirotetramat residues in ora nge juice and prunes. Samples of orange juice and prun e fruit were spiked individually with 0.20 ppm of e ach spirotetramat, BYI 08330-enol, BYI 08330-ketohydro xy, BYI 08330-monohydroxy, BYI 08330-enol-Glc and stored at <-18oC. Spiked samples were analyzed usin g method 00857 (LC-MS/MS method) at 0-, 30-, 90-, and 144/147-day intervals.

Findings : A summary of the % corrected recoveries and % decli ne expressed as spirotetramat equivalents can be found in table B.7.6.12.1-1.- 134 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Table B.7.6.12.1-1: Summary of Concurrent Recoveries of Spirotetramat and Metabolites from Plant Matrices.Spirotetramat BYI 08330-EnolBYI 08330-KetohydroxyBYI 8330-MonohydroxyBYI 08330-Enol-GlcMatrixSpikelevel(mg/kg)StorageInterval(days)Samplesize(n)Recovery(%)AverageRecovery(%)Recovery(%)AverageRecovery(%)Recovery(%)AverageRecovery(%)Recovery(%)AverageRecovery(%)Recovery(%)AverageRecovery(%)0.01 0 2 99, 100 100 105, 109 107 90, 105 98 94, 103 99 91, 101 960.2 32 2 91, 77 84 88, 72 86 95, 80 88 89, 73 81 91, 75 830.2 62 2 99, 94 97 97, 91 94 96, 92 94 103, 101 10298, 93 960.2 91 2 73, 98 86 72, 103 87 74, 101 88 74, 97 8570, 95 830.01 2 92, 90 91 95, 97 96 104, 107 106 100, 95 98108, 103 1060.21802 73, 77 75 80, 85 83 87, 94 91 77, 86 82 77, 84 810.01 2 103, 72 88 103, 78 91 98, 74 86 108, 80 94 109, 80 950.23702 85, 104 95 86, 101 94 86, 96 91 86, 98 92 84, 102930.01 2 93, 90 92 91, 86 89 102, 95 99 93, 88 91 93,85 890.25432 90, 90 90 89, 90 90 95, 94 95 87, 89 88 89, 91 900.01 2 106, 94 100 103, 105 104 96, 96 96 98, 101 100 103, 105 104Tomato(fruit)0.27182 97, 86 92 97, 87 92 83, 93 88 96, 84 90 97, 87 920.01 0 2 73, 85 79 76, 96 86 86, 84 85 76, 89 83 70, 80 750.2 31 2 98, 96 97 93, 93 93 104, 103 104 97, 94 96104, 96 1000.2 62 2 75, 94 85 74, 88 81 78, 93 86 83, 95 89 69, 83 760.2 90 2 61, 85 73 64, 84 74 64, 90 77 66, 88 77 65, 90 780.01 2 89, 71 80 96, 82 89 112, 79 96 100, 88 94 107, 84 960.21802 86, 79 83 103, 93 98 107, 91 99 106, 95 101 102,90 960.01 2 120, 97 109 98, 86 92 92, 82 87 105, 93 99 101, 86 940.23702 82, 98 90 79, 104 92 81, 99 90 84, 103 94 74, 96850.01 2 65, 102 84 70, 87 79 65, 95 80 64, 100 82 62, 96 790.25432 101, 101 101 100, 99 100 99, 100 100 101, 101 10197, 100 990.01 2 105, 100 103 105, 100 103 107, 100 104 97, 100 99 105, 100 103Potato(tuber)0.27172 96, 82 89 93, 79 86 95, 81 88 95, 75 85 93, 79 860.01 0 2 94, 88 91 98, 93 96 90, 91 91 96, 89 92 99, 92 960.2 29 2 103, 99 101 96, 92 94 107, 102 105 96, 9495 103, 93 980.2 62 2 96, 85 91 93, 85 89 93, 89 91 95, 86 90 91, 83 870.2 90 2 102, 103 103 104, 99 101 100, 98 99 99, 9898 104, 109 1070.01 2 96, 81 89 101, 84 93 98, 77 88 102, 84 93 100, 83 92Lettuce(head)0.21772 92, 80 86 100, 87 94 102, 85 99 100, 89 94 97, 8491- 135 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Spirotetramat BYI 08330-EnolBYI 08330-KetohydroxyBYI 8330-MonohydroxyBYI 08330-Enol-GlcMatrixSpikelevel(mg/kg)StorageInterval(days)Samplesize(n)Recovery(%)AverageRecovery(%)Recovery(%)AverageRecovery(%)Recovery(%)AverageRecovery(%)Recovery(%)AverageRecovery(%)Recovery(%)AverageRecovery(%)0.01 2 90, 94 92 90, 91 91 86, 95 91 99, 100 100 91, 100 960.23662 96, 86 91 90, 82 86 89, 79 84 95, 85 90 93, 79 860.01 541 2 95, 98 97 91, 97 94 97, 93 95 106, 114 110 94, 101 980.2 2 97, 99 98 94, 96 95 95, 97 96 102, 98 100 101, 100 1010.01 2 92, 95 94 84, 88 88 89, 94 92 94, 93 94 88,88 880.27132 96, 104 100 94, 98 96 101, 107 104 98, 103 101 94, 98 960.01 0 2 70, 92 81 83, 102 9368,8275 75, 99 87 73, 101 870.2 28 2 93, 95 94 84, 85 85 101, 103 102 88, 88 8888, 90 890.2 60 2 82, 79 81 79, 75 77 87, 84 86 91, 84 88 87, 79 830.2 91 2 98, 95 97 91, 89 90 98, 90 94 102, 92 97 102, 88 950.01 2 86, 95 91 101, 98 100 96, 96 96 97, 96 96 116, 120 1180.21772 67, 87 77 73, 102 88 72, 98 85 73, 101 87 73, 103880.01 2 89, 91 90 87, 92 90 91, 107 99 86, 89 88 86,84 850.23672 92, 73 83 92, 71 82 101, 78 90 89, 68 78 91, 71 810.01 2 89, 92 91 84, 91 88 90, 97 94 99, 105 102 84, 88 860.25422 94, 76 85 89, 72 81 89, 72 81 97, 78 88 95, 75 850.01 2 85, 100 93 75, 95 85 79, 102 91 80, 99 90 75, 95 80ClimbingFrenchBean(beanwith pod)0.27142 88, 89 89 87, 83 85 90, 91 91 88, 87 88 87, 83 850.01 0 2 103, 104 104 106, 103 105 98, 101 100 99,101 100 98, 89 940.2 26 2 101, 103 102 94, 95 95 109, 109 109 96, 9897 102, 101 1020.2 61 2 101, 101 101 100, 97 99 104, 105 105 103,106 104 98, 95 970.2 90 2 95, 95 95 102, 100 101 97, 101 99 99, 100100 99, 103 1010.01 2 85, 90 88 85, 97 91 94, 93 94 94, 93 94 89,96 930.21772 91, 94 93 97, 94 96 103, 105 104 105, 100 102 102, 98 1000.01 2 89, 88 90 99, 95 97 100, 100 100 93, 99 96 101, 94 980.23672 90, 81 86 98, 84 91 93, 85 89 94, 83 88 91, 84 880.01 2 89, 90 90 91, 97 94 100, 90 95 103, 108 10694, 92 930.25412 84, 92 88 93, 99 96 93, 99 96 91, 95 93 85, 90 880.01 2 84, 83 84 83, 85 84 82, 82 82 86, 84 85 87,87 87Almond(nutmeat)0.27132 84, 87 86 86, 88 87 87, 88 88 88, 89 89 86, 90 880.01 0 2 100, 99 100 75, 76 76 100, 98 99 102, 102102 101, 101 101Tomato(paste)0.2 30 2 89, 84 87 89, 84 87 96, 90 93 95, 92 94 86, 85 86- 136 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Spirotetramat BYI 08330-EnolBYI 08330-KetohydroxyBYI 8330-MonohydroxyBYI 08330-Enol-GlcMatrixSpikelevel(mg/kg)StorageInterval(days)Samplesize(n)Recovery(%)AverageRecovery(%)Recovery(%)AverageRecovery(%)Recovery(%)AverageRecovery(%)Recovery(%)AverageRecovery(%)Recovery(%)AverageRecovery(%)0.2 61 2 96, 97 97 106, 111 109 103, 96 99 105, 108107 102, 104 1030.2 93 2 91, 101 96 101, 101 101 95, 103 99 99, 100100 96, 96 960.01 2 101, 101 101 96, 98 97 92, 82 99 93, 101 9796, 95 960.21872 90, 103 97 94, 101 98 88, 97 93 90, 93 92 86, 92890.01 2 95, 99 97 103, 91 97 97, 94 96 92, 91 92 80,81 810.23732 96, 90 93 98, 95 97 94, 89 92 97, 91 94 96, 92 940.01 2 90, 81 86 84, 76 80 97, 82 90 89, 81 85 82,85 840.25422 92, 94 93 87, 87 87 95, 96 96 89, 89 89 89, 90 900.01 715 2 93, 101 97 95, 99 97 99, 95 97 98, 92 9587, 91 890.2 2 96, 98 97 100, 101 101 95, 97 96 90, 95 93 86, 90 880.01 3 104, 97,98100 102, 100,101101 89, 91, 97 92 93, 90, 89 91 93, 90, 89 910.203 104, 90,10299 101, 88,10096 87, 91, 94 91 88, 89, 91 89 88, 89, 91 890.2 30 2 74, 91 83 76, 94 85 72, 90 81 68, 87 78 68, 87 780.2 92 2 99, 96 98 108, 103 105 108, 103 106 102, 98 100 102, 98 100Orange(juice)0.2 144 2 93, 86 89 100, 91 95 117, 98 108 87, 86 86 87, 86 870.01 3 101, 101,97100 101, 98,9598 82, 86, 87 85 90, 87, 83 87 90, 87, 83 870.203 96, 96,10097 96, 94,10097 86, 84, 83 84 85, 87, 86 86 85, 87, 86 860.2 30 2 90, 95 93 91, 94 93 92, 91 92 90, 98 94 90, 98 940.2 92 2 101, 101 101 99, 97 98 83, 88 86 94, 94 9494, 94 94Prunes(fruit)0.2 147 2 94, 95 94 105, 100 102 103, 98 101 103, 93 98 103, 93 98

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Samples spiked with spirotetramat were analyzed for all analytes and the total residues were expressed as BYI08330 equivalents.Total spirotetramat residues w ere stable (<30% degradation) in all matrices durin g freezer storage for up to 718 days. Total BYI08330- enol residues declined by 35% in tomato paste after 715 days of freezer storage. Residues of BYI 08330-keto hydroxy, -mono-hydroxy and -enol-Glc were stable (<30% degradation) in all matrices analyzed for up to 718 days (see Table B.7.6.12.1-2).

Table B.7.6.12.1-2: Summary of the Stability of Tot al Residues of Spirotetramat (BYI 08330) in Plant Matrices Following Storage at -18°C.

Total Spirotetra mat Residues Commodity Spiking level

(mg/kg) Storage interval

(days) n

mg/kg % uncorrected recovery %

corrected recovery* % decline

0 5 0.189 95 95 5

32 3 0.202 101 121 --

62 3 0.171 86 89 11

91 3 0.184 92 107 --

180 3 0.173 87 115 --

370 3 0.177 89 93 7

543 3 0.187 94 104 -- Tomato Fruit 0.2

718 3 0.185 93 101 --

0 5 0.178 89 112 --

31 3 0.196 98 101 --

62 3 0.168 84 99 1

90 3 0.150 76 103 --

180 3 0.196 98 118 --

370 3 0.183 92 102 --

543 3 0.137 69 68 32 Potato Tuber 0.2

717 3 0.171 86 96 4

0 5 0.167 84 92 8

29 3 0.193 97 96 4

62 3 0.197 99 108 --

90 3 0.183 92 89 11

177 3 0.183 92 106 --

366 3 0.192 96 105 --

541 3 0.190 95 97 3 Head lettuce 0.2

713 3 0.185 93 93 7

0 5 0.179 90 110 --

28 3 0.176 88 94 6

60 3 0.173 87 107 --

91 3 0.180 90 93 7

177 3 0.189 95 123 --

367 3 0.211 106 127 --

542 3 0.164 82 96 4 Climbing French bean 0.2

714 3 0.170 85 98 2

0 5 0.169 85 85 15

26 3 0.217 109 109 --

61 3 0.202 101 101 --

90 3 0.190 95 100 --

177 3 0.187 94 101 --

367 3 0.176 88 102 --

541 3 0.179 90 102 -- Almond nutmeat 0.2

713 3 0.168 84 98 2

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Total Spirotetra mat Residues Commodity Spiking level

(mg/kg) Storage interval

(days) n

mg/kg % uncorrected recovery %

corrected recovery* % decline

0 5 0.208 104 104 --

30 3 0.200 100 115 --

61 3 0.200 100 103 --

93 3 0.198 99 103 --

187 3 0.165 83 85 15

373 3 0.175 88 94 6

542 3 0.191 96 103 -- Tomato Paste 0.2

715 3 0.183 92 94 6

0 5 0.197 99 99 1

30 3 0.147 74 89 11

92 3 0.179 89 91 9 Orange juice 0.2

144 3 0.191 96 107 --

0 5 0.193 97 99 1

30 3 0.139 70 75 25

92 3 0.171 86 86 14 Prunes 0.2

147 3 0.166 83 88 12 

### * Corrected for mean concurrent recovery (see Table B.7.6.12.1-1).

Total residues of spirotetramat in orange juice and prunes were stable (<30% degradation) during froze n storage for up to 147 days.

Conclusion:

There are adequate storage stability data to valida te the storage conditions and intervals of samples collected from the field trial studies.

B.7.7 Effects of industrial processing and/or house hold preparation (Annex IIA 6.5; Annex

IIIA 8.5)

B.7.7.1 Effects on the nature of the residue

B.7.7.1.1 BYI 08330

Reference: BYI 08330: Aqueous hydrolysis under conditions of p rocessing studies Author(s), year: Koch, Sur; 2005, amended April 200 6 Report/Doc. number: MEF-04/562 M-269158-02-1 Guideline(s): EU Council Directive 91/414/EEC as am ended by Commission Directive 96/68/EC Section 6.5, Subsection 6.5.1. Guideline 7035/VI/95 Revision 5, Appendix E (July 1997) GLP: Yes. Deviations: None. Validity: The study is considered acceptable.

The purpose of this study was to describe the degra dation behaviour of the insecticide spirotetramat ( BYI 08330) in buffered drinking water. The experiments were carried out under laboratory conditions which are representative for processing operations of raw agr icultural commodities.

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Material and methods: The experiments were performed with two different c oncentrations. [Azaspirodecenyl-3- 14 

### C]FHN 12952 (BYI 08330) was applied at two different projected doses of 0.2 mg a.s./L (experiment 1) and of 1.0 mg a.s. /L (experiment 2) buffer solution. To simulate the con ditions of processing studies, non-sterilized drink ing water was used. The test systems were incubated at three representative sets of hydrolysis conditions:

Pasteurisation: 90 °C at pH 4 for 20 min (water bat h); Baking, brewing, boiling: 100 °C at pH 5 for 60 min (water bath); and Sterilisation: 120 °C at pH 6 for 20 min (autoclave ).

The pH was adjusted to and remained at pH 4, pH 5 a nd pH 6 (each ± 0.2) as required. The temperatures were in the required ranges of 90 ± 3 °C (89.9-90.2 °C), 100 ± 3 °C (97.8 to 99.8) and 120 ± 3 °C durin g the test periods. The periods for heating and cooling t o the required temperatures prior to and after the incubation, respectively, were not regarded as test periods. The test period started, when the require d temperature was reached and was terminated by cooli ng down, when the test time was over.

At time zero (test start) and at test termination, the content of radioactivity was determined in the samples by liquid scintillation counting. Parent compound and hydrolysis product were identified and quantified b y HPLC. For the HPLC method, the detection limit of compone nts in the test solutions was determined. The LOD i s defined as a signal which is 2.5 to 3 times the Sig nal/Noise ratio. The detection limit meets the requ irement of the guideline, where identification is asked for hydrolysis products in concentrations higher or eq ual to 0.05 mg/kg. The calculated recovery was 99.9%. Sinc e no radioactivity remained on the column, the HPLC

method was proven to be valid for the analysis of t he samples. Thin layer chromatography (TLC) was used as second method for identification of active substance and hydrolysis product by co-chromatography with non la belled reference items.

Findings: The applied radioactivity was defined as the amount of radioactivity measured in the subsamples taken at the beginning of the incubation period. Based on th e results of LSC measurements immediately after tes t termination, a radioactivity balance was establishe d for each experiment. The material balances ranged from 100.0% to 111.4% of the applied radioactivity for e xperiment 1 and from 102.5% to 107% for experiment 2. The material balances demonstrate that no radioacti vity and no volatile decomposition product dissipat ed from the test system. The concentration effect is d ue to increasing evaporation of water from the test system with increasing temperature. Quantitative analysis and identification of the act ive substance and the hydrolysis product by cochromatography was performed by HPLC for all sample s.

At zero-time, the active substance BYI 08330 was st able and amounted to between 99.5% and 100% of the applied radioactivity (AR) for both experiments. Du ring the treatment the active substance degraded to BYI 08330-enol (reference item code: A1302944) in diffe rent amounts, depending on the pH value. At pH 4 / 90°C the active substance is stable (experiment 1: 98.0% of the AR; experiment 2: 98.1% of the AR). At pH=5 / 100°C a degradation of ca. 15% is found (exp eriment 1: BYI 08330 is 84.5% of the AR; experiment 2: BYI 08330 is 86.0% of the AR). At pH=6 / 120°C the degradation was nearly complete. The active substan ce decreased to 14.6% of the AR (experiment 1) and 16. 3% of the AR (experiment 2). Identification of the active substance and of BYI 08330-enol was performed by HP LC co-chromatography with the non-labelled reference item for all samples. No further hydrolys is products or degradation products were found. The quantification of BYI 08330 and BYI 08330-enol in the test solutions is presented in Table B.7.7.1 .1-1:

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.7.1.1-1: Quantification of BYI 08330 and BYI 08330-enol in the samples of experiment 1 and experiment 2 by HPLC [expressed as percentage of ap plied radioactivity: Experiment 1 (0.2 mg a.s./L) Experiment 2 (1 mg a.s./L) compound BYI 08330 BYI 08330-enol BYI 08330 BYI 08330-e nol

time pH

/ temp. Area% 1) Mean%

2) Area%

1) Mean%

2) Area%

1) Mean%

2) Area%

1) Mean%

2)

pH=4 90 °C 100.0

99.5 99.7 0.0 0.5 0.3 100.0 100.0 100.0 0.0 0.0 0.0

pH=5 100 °C 99.5

99.5 99.5 0.5 0.5 0.5 100.0 100.0 100.0 0.0 0.0 0.0 Zero time

pH=6

120 °C 99.0

100.0 99.5 1.0 0.0 0.5 100.0 99.5 99.7 0.0 0.5 0.3

pH=4 90 °C 98.1

97.8 98.0 1.9 2.2 2.0 98.4 97.8 98.1 1.6 2.2 1.9

pH=5 100 °C 84.7

84.3 84.5 15.3 15.7 15.5 86.3 85.8 86.0 13.7 14.3 14.0 Test termination

pH=6

120 °C 14.6

14.6 14.6 85.4 85.4 85.4 16.2 16.5 16.3 83.8 83.5 83.7

1) Area% of HPLC analysis

2) Area% mean value of two samples 

### TLC was used as second analytical method for identi fication of the active substance and of the degrada tion product BYI 08330-enol by co-chromatography. No fur ther hydrolysis products or degradation products we re found.

Conclusion: BYI 08330 (spirotetramat) is hydrolysed under condi tions being representative for processing studies. At conditions of pH=4 / 90°C (20 min) representing pasteurisation

, no significant hydrolysis was found. At pH=5 / 100 °C (60 min) ca. 15% degradation was obse rved. At conditions of pH=6 / 120 °C (20 min) representing sterilisation , the active substance degraded nearly completely (ca. 85%). BYI 08330-enol was found as the only hydrolysis product formed.

B.7.7.1.2 BYI 08330-enol

Reference: BYI 08330-enol: Aqueous hydrolysis under conditions of processing studies Author(s), year: Koch, Sur; 2006 Report/Doc. number: MEF-05/227 M-267011-01-1 Guideline(s): EU Council Directive 91/414/EEC as am ended by Commission Directive 96/68/EC Section 6.5, Subsection 6.5.1. Guideline 7035/VI/95 Revision 5, Appendix E (July 1997) GLP: Yes. Deviations: None. Validity: The study is considered acceptable.

The purpose of this study was to describe the degra dation behaviour of the BYI 08330-enol in buffered drinking water. The experiments were carried out un der laboratory conditions which are representative for processing operations of raw agricultural commoditi es.

Material and methods: The experiments were performed with two different c oncentrations. [Azaspirodecenyl-3- 14 

### C]cis-BYI 08330- enol was applied at two different projected doses o f 0.2 mg a.s./L (experiment 1) and of 1.0 mg a.s./L

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

(experiment 2) buffer solution. To simulate the con ditions of processing studies, non-sterilized drink ing water was used. The test systems were incubated at three representative sets of hydrolysis conditions:

Pasteurisation: 90 °C at pH 4 for 20 min (water bat h); Baking, brewing, boiling: 100 °C at pH 5 for 60 min (water bath); and Sterilisation: 120 °C at pH 6 for 20 min (autoclave ).

The pH was adjusted to and remained at pH 4, pH 5 a nd pH 6 (each ± 0.2) as required. The temperatures were in the required ranges of 90 ± 3 °C (90.1°C), 100 ± 3 °C (100.1) and 120 ± 3 °C during the test p eriods. The periods for heating and cooling to the required temperatures prior to and after the incubation, respectively, were not regarded as test periods. Th e test period started, when the required temperatur e was reached and was terminated by cooling down, when th e test time was over.

At time zero (test start) and at test termination, the content of radioactivity was determined in the samples by liquid scintillation counting. Parent compound and hydrolysis product were identified and quantified b y HPLC. By the time of the beginning of the present study s everal analytical works on metabolism of BYI 08330 has already been reported; in these studies the recover y of a.i. and metabolites in several HPLC systems is described. During the work on these studies no evid ence had been observed that the test item or one of the hydrolysis products are not completely recovered af ter chromatography. Therefore, no further work was done to reinvestigate the recovery of this HPLC method. For the HPLC system, the detection limit (LOD) is expressed as minimum area required for a peak, The LOD expressed as % of the injected RA (radioactivit y) was calculated. For experiment A the LOD was in the range from 0.9% to 1.2%, for experiment B the LOD was ≤1% for all chromatograms.

Findings: The applied radioactivity was defined as the amount of radioactivity measured in the subsamples taken at the beginning of the incubation period. Based on th e results of LSC measurements immediately after tes t termination, a radioactivity balance was establishe d for each experiment. The material balances ranged from 103.0% to 104.8% of the applied radioactivity for e xperiment 1 and from 103.6% to 112.2% for experimen t 2. The material balances demonstrate that no radioacti vity and no volatile decomposition product dissipat ed from the test system. The concentration effect is d ue to increasing evaporation of water from the test system with increasing temperature. Quantitative analysis and identification by co-chro matography was performed by HPLC for all samples. BYI 08330-enol remained unaffected under all tested conditions. In none of the sample s hydrolysis products were found. The measured radioactivity in test solutions is pre sented in Table B.7.7.1.2-1:

Table B.7.7.1.2-1: Measured radioactivity in test s olutions: Experiment 1 (0.2 mg a.s./L) Experiment 2 (1 mg a.s./L) compound BYI 08330-enol BYI 08330-enol

time pH

/ temp. Total

[Bq] Mean

Total [Bq] samples Test item

equivalents [μg/L] 1) Total

[Bq] Mean

Total [Bq] samples Test item

equivalents [μg/L] 1)

pH=4 90 °C 5271.5

5256.0 5264 231.9 23950.0 21339.0 22645 997.6

pH=5 100 °C 4975.0

5245.0 5110 225.1 22870.0 24094.0 23482 1034.4 Zero time

pH=6

120 °C 5151.5

5203.0 5177 228.1 21932.5 24196.5 23065 1016.1

Test termination pH=4

90 °C 5328.0

5512.5 5420 238.8 22334.0 24574.0 23454 1033.2

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Experiment 1 (0.2 mg a.s./L) Experiment 2 (1 mg a.s./L) compound BYI 08330-enol BYI 08330-enol

time pH

/ temp. Total

[Bq] Mean

Total [Bq] samples Test item

equivalents [μg/L] 1) Total

[Bq] Mean

Total [Bq] samples Test item

equivalents [μg/L] 1)

pH=5 100 °C 5281.0

5244.0 5263 231.8 24311.0 25183.5 24747 1090.2

pH=6 120 °C 5412.5

5440.0 5426 239.0 25786.0 25964.5 25875 1139.9

1) Calculation: [Mean Total (Bq) / specific activity: 4540 Bq/ μ g] / (processing volume: 0.005 L)



### Conclusion: BYI 08330-enol was found to be resistant to hydroly sis under conditions being representative for processing studies. At conditions of pH=4 / 90°C (2 0 min) as well as at conditions of pH=5 / 100 °C (6 0 min) and at conditions of pH=6 / 120 °C (20 min) BYI 083 30-enol remained unchanged. This result is in accordance to the finding in the processing study o f BYI 08330 (parent spirotetramat): under condition s of processing studies BYI 08330 was hydrolyzed to BYI 08330-enol, but no further degradation products wer e formed (see B.7.7.1.1). Therefore, hydrolysis does not affect the nature of BYI 08330-enol residues during raw agricultural commodity processing operations.

B.7.7.1.3 BYI 08330-enol-glucoside

Reference: BYI 08330-enol-glucoside: Aqueous hydrolysis under conditions of processing studies Author(s), year: Koch, Sur; 2006 Report/Doc. number: MEF-05/274 M-266907-01-1 Guideline(s): EU Council Directive 91/414/EEC as am ended by Commission Directive 96/68/EC Section 6.5, Subsection 6.5.1. Guideline 7035/VI/95 Revision 5, Appendix E (July 1997) GLP: Yes. Deviations: None. Validity: The study is considered acceptable.

The purpose of this study was to describe the degra dation behaviour of the BYI 08330-enol-glucoside in buffered drinking water. The experiments were carri ed out under laboratory conditions which are representative for processing operations of raw agr icultural commodities.

Material and methods: The experiments were performed with two different c oncentrations. [Azaspirodecenyl-3- 14 

### C]-BYI 08330-enolglucoside was applied at two different projected do ses of 0.2 mg a.s./L (experiment 1) and of 1.0 mg a .s./L (experiment 2) buffer solution. To simulate the con ditions of processing studies, non-sterilized drink ing water was used. The test systems were incubated at three representative sets of hydrolysis conditions:

Pasteurisation: 90 °C at pH 4 for 20 min (water bat h); Baking, brewing, boiling: 100 °C at pH 5 for 60 min (water bath); and Sterilisation: 120 °C at pH 6 for 20 min (autoclave ).

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The pH was adjusted to and remained at pH 4, pH 5 a nd pH 6 (each ± 0.2) as required. The temperatures were in the required ranges of 90 ± 3 °C (89.9 to 8 9.95°C), 100 ± 3 °C (99.85 to 100.0 °C) and 120 ± 3 °C during the test periods. The periods for heating an d cooling to the required temperatures prior to and after the incubation, respectively, were not regarded as test periods. The test period started, when the req uired temperature was reached and was terminated by cooli ng down, when the test time was over.

At time zero (test start) and at test termination, the content of radioactivity was determined in the samples by liquid scintillation counting. Parent compound and hydrolysis product were identified and quantified b y HPLC. By the time of the beginning of the present study s everal analytical works on metabolism of BYI 08330 has already been reported; in these studies the recover y of a.i. and metabolites in several HPLC systems is described. During the work on these studies no evid ence had been observed that the test item or one of the hydrolysis products is not completely recovered aft er chromatography. Therefore, no further work was d one to reinvestigate the recovery of this HPLC method. For the HPLC method, the detection limit of compone nts in the test solutions was determined yet (see B.1.7 .1.1). The LOD is defined as a signal which is 2.5 to 3 times the signal/noise ratio. The LOD was <1% of th e applied radioactivity for all chromatograms. The detection limit meets the requirement of the guidel ine, where identification is asked for hydrolysis p roducts in concentrations higher or equal to 0.05 mg/kg.

Findings: The applied radioactivity was defined as the amount of radioactivity measured in the subsamples taken at the beginning of the incubation period. Based on th e results of LSC measurements immediately after tes t termination, a radioactivity balance was establishe d for each experiment. The material balances ranged from 103.1% to 104.8% of the applied radioactivity for e xperiment 1 and from 100.3% to 103.3% for experimen t 2. The material balances demonstrate that no radioacti vity and no volatile degradation products dissipate d from the test system. The concentration effect is due to the evaporation of water from the test system duri ng processing. The test item was hydrolysed to BYI 08330-enol in d ifferent amounts, depending on the processing conditions. BYI 08330-enol-glucoside was demonstrat ed to be resistant to hydrolysis under conditions b eing representative for pasteurisation. Under conditions representative for baking, brewing and boiling a degradation of ca. 10% was found. Under conditions of sterilisation ca. 40% of the test item were hydr olysed. BYI 08330-enol was found as the only hydrolysis pro duct. The quantification of BYI 08330-enol-glucoside and BYI 08330-enol in the test solutions is presented i n Table B.7.7.1.3-1.

Table B.7.7.1.3-1: Quantification of BYI 08330-enol -glucoside and BYI 08330-enol in the samples of experiment 1 and experiment 2 by HPLC [expressed as percentage of applied radioactivity]: Experiment 1 (0.2 mg a.s./L) Experiment 2 (1 mg a.s./L)

compound BYI 08330-enolglucoside BYI 08330-enol BYI 08330-enolglucoside BYI 08330-enol

time pH

/ temp. Area% 1) Mean%

2) Area%

1) Mean%

2) Area%

1) Mean%

2) Area%

1) Mean%

2)

pH=4 90 °C 100.0

100.0 100.0 0.0 0.0 0.0 100.0 100.0 100.0 0.0 0.0 0.0

pH=5 100 °C 100.0

100.0 100.0 0.0 0.0 0.0 100.0 100.0 100.0 0.0 0.0 0.0 Zero time

pH=6

120 °C 100.0

100.0 100.0 0.0 0.0 0.0 100.0 100.0 100.0 0.0 0.0 0.0

pH=4 90 °C 98.4

98.2 98.3 1.7 1.8 1.7 98.4 98.6 98.5 1.7 1.5 1.6 Test termination pH=5

100 °C 91.9

92.2 92.1 8.1 7.8 7.9 89.3 89.9 89.9 10.7 10.1 10.4

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Experiment 1 (0.2 mg a.s./L) Experiment 2 (1 mg a.s./L)

compound BYI 08330-enolglucoside BYI 08330-enol BYI 08330-enolglucoside BYI 08330-enol

time pH

/ temp. Area% 1) Mean%

2) Area%

1) Mean%

2) Area%

1) Mean%

2) Area%

1) Mean%

2)

pH=6 120 °C 58.7

58.0 58.3 41.3 42.0 41.7 58.6 58.2 58.4 41.4 41.8 41.6

1) Calculation: [Mean Total (Bq) / specific activity: 2990 Bq/ μ g] / (processing volume: 0.005 L)

2) Calculation: [Mean Total (Bq) / specific activity: 639 Bq/ μ g] / (processing volume: 0.005 L)



### Conclusion: BYI 08330-enol-glucoside was found to be hydrolysed under certain conditions being representative for processing studies. At conditions of pH=4 / 90 °C ( 20 min) no significant hydrolysis was found. At pH= 5 / 100 °C (60 min) ca. 10% degradation was observed. At co nditions of pH=6 / 120 °C (20 min) ca. 40% degradation was found. BYI 08330-enol was the only hydrolysis product form ed

.

B.7.7.1.4 BYI 08330-keto-hydroxy

Reference: BYI 08330-keto-hydroxy: Aqueous hydrolysis under co nditions of processing studies Author(s), year: Koch, Sur; 2006 Report/Doc. number: MEF-05/409 M-267024-01-1 Guideline(s): EU Council Directive 91/414/EEC as am ended by Commission Directive 96/68/EC Section 6.5, Subsection 6.5.1. Guideline 7035/VI/95 Revision 5, Appendix E (July 1997) GLP: Yes. Deviations: None. Validity: The study is considered acceptable.

The purpose of this study was to describe the degra dation behaviour of the BYI 08330-keto-hydroxy in buffered drinking water. The experiments were carri ed out under laboratory conditions which are representative for processing operations of raw agr icultural commodities.

Material and methods: The experiments were performed with two different c oncentrations. [Azaspirodecenyl-3- 14 

### C]FHN-14066 (BYI 08330-keto-hydroxy) was applied at two different pr ojected doses of 0.2 mg a.s./L (experiment 1) and o f 1.0 mg a.s./L (experiment 2) buffer solution. To simula te the conditions of processing studies, non-steril ized drinking water was used. The test systems were incu bated at three representative sets of hydrolysis conditions:

Pasteurisation: 90 °C at pH 4 for 20 min (water bat h); Baking, brewing, boiling: 100 °C at pH 5 for 60 min (water bath); and Sterilisation: 120 °C at pH 6 for 20 min (autoclave ).

The pH was adjusted to and remained at pH 4, pH 5 a nd pH 6 (each ± 0.2) as required. The temperatures were in the required ranges of 90 ± 3 °C (89.9 to 9 0.3°C), 100 ± 3 °C (100.0 to 100.8 °C) and 120 ± 3 °C (120 to 121.4 °C) during the test periods. The peri ods for heating and cooling to the required tempera tures prior to and after the incubation, respectively, we re not regarded as test periods. The test period st arted,

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when the required temperature was reached and was t erminated by cooling down, when the test time was

over. The 14 

### C-radioactivity of liquid samples was determined by liquid scintillation counting (LSC). Parent compound and hydrolysis product were identified and quantified by HPLC. By the time of the beginning o f the present study analytical work on aqueous hydrol ysis under conditions of processing studies of BYI 08330 had already been finished (see B.7.7.1.1). In these studies the quantitative recovery of the active su bstance and metabolites is described using the similar HPLC method. Therefore no work was done to reinvestigat e the recovery of this HPLC method. For the HPLC meth od a detection of 1% of the injected radioactivity is required: In the HPLC-chromatograms peaks of <1 are a% were detectable. The detection limit meets the requirement of the guideline, where identification is asked for hydrolysis products in concentrations higher or equal to 0.05 mg/kg. Thin layer chromatography was used for identificati on of test item by co-chromatography with non label led reference standards. During the treatment the test item hydrolysed to BY I 08330-MA-amide. The structure of the compound was elucidated by NMR and MS techniques after isolation by HPLC.

Findings: The applied radioactivity was defined as the amount of radioactivity measured in the subsamples taken at the beginning of the incubation period. Based on th e results of LSC measurements immediately after tes t termination, a radioactivity balance was establishe d for each experiment. The material balances ranged from 100.3% to 106.5% of the applied radioactivity for e xperiment 1 and from 101.1% to 102.2% for experimen t 2. The material balances demonstrate that no radioacti vity and no volatile degradation products dissipate d from the test system. The concentration effect is due to the evaporation of water from the test system duri ng processing. The measured radioactivity in test solutions is pre sented in Table B.7.7.1.4-1.

Table B.7.7.1.4-1: Measured radioactivity in test s olutions: Experiment 1 (0.2 mg a.s./L) Experiment 2 (1 mg a.s./L) compound BYI 08330- keto-hydroxy BYI 08330- keto-hydr oxy

time pH

/ temp. Total

[Bq] Mean

Total [Bq] samples Test item

equivalents [μg/L] 1) Total

[Bq] Mean

Total [Bq] samples Test item

equivalents [μg/L] 1)

pH=4 90 °C 4332.9

4476.7 4405 204.4 21705.00 22388.33 22047 1023.0

pH=5 100 °C 4358.3

4473.8 4416 204.9 22098.33 22406.67 22253 1032.6 Zero time

pH=6

120 °C 4006.7

4373.3 4190 194.4 21865.00 22028.33 21947 1018.4

pH=4 90 °C 4327.5

4515.0 4421 205.2 22075.00 22505.00 22290 1034.3

pH=5 100 °C 4382.1

4473.8 4428 205.5 22385.00 22680.00 22533 1045.6 Test termination

pH=6

120 °C 4421.7

4501.3 4461 207.0 22410.00 22443.33 22427 1040.7

1) Calculation: [Mean Total (Bq) / specific activity: 4310 Bq/ μ g] / (processing volume: 0.005 L)



### At zero-time, the test item BYI 08330-keto-hydroxy was stable and amounted to between 99.5% and 99.8% of the applied radioactivity for experiment 1 and t between 99.4% and 99.6% of the applied radioactivi ty for experiment 2 (see Table B.7.7.1.4-2). During the tr eatment the test item hydrolysed to BYI 08330-MAamide . The amount of degradation depended on the pH valu e. At pH 4 / 90°C the test item was stable (experiment 1: 99.5% of the AR; experiment 2: 99.5% of the AR). At pH=5 / 100°C a degradation of ca. 5 % is found (experiment 1: BYI 08330-keto-hydroxy is 95.4 % of the AR; experiment 2: BYI 08330-keto-hydroxy i s

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

95.3% of the AR). At pH=6 / 120°C the degradation w as nearly complete. The test item decreased to 0.9% of the AR (experiment 1) and 0.5% of the AR (experimen t 2). A minor hydrolysis product was detected in both experiments at pH=6 / 120°C ( retention time: 36.5 min). Because of the low amount (mean content <1% of AR) no characterisation work was spent on this compound. No further hydrolysis products or degradation produ cts were found.

Table B.7.7.1.4-2: Quantification of BYI 08330-keto -hydroxy and BYI 08330-MA-amide in the samples of experiment 1 (top) and experiment 2 (bottom) byH PLC

BYI 08330- ketohydroxy 1) BYI 08330-MA-amide 1) Unknown 1) Experiment 1 (0.2 mg a.s./L) Area% 2) Mean% 3) Area% 2) Mean% 3) Area% 2) Mean% 3)

pH=4 90 °C 99.5

99.5 99.5 0.5 0.5 0.5 ---

--- ---

pH=5 100 °C 99.6

99.5 99.6 0.4 0.5 0.4 ---

--- --- Zero time

pH=6

120 °C 99.6

100.0 99.8 0.4 0.0 0.2 ---

--- ---

pH=4 90 °C 99.5

99.5 99.5 0.5 0.5 0.5 ---

--- ---

pH=5 100 °C 95.4

95.4 95.4 4.6 4.6 4.6 ---

--- --- Test termination

pH=6

120 °C 1.3

0.6 0.9 98.3 99.0 98.6 0.4 0.4 0.4

BYI 08330- ketohydroxy 1) BYI 08330-MA-amide 1) Unknown 1) Experiment 2 (1 mg a.s./L) Area% 2) Mean% 3) Area% 2) Area%

2) Mean% 3) Area% 2)

pH=4 90 °C 99.6

99.4 99.5 0.4 0.6 0.5 ---

--- ---

pH=5 100 °C 99.4

99.5 99.4 0.6 0.5 0.6 ---

--- --- Zero time

pH=6

120 °C 99.6

99.5 99.6 0.4 0.5 0.4 ---

--- ---

pH=4 90 °C 99.5

99.5 99.5 0.5 0.5 0.5 ---

--- ---

pH=5 100 °C 95.5

95.1 95.3 4.6 4.9 4.7 ---

--- --- Test termination

pH=6

120 °C 0.5

0.5 0.5 98.9 99.1 99.0 0.6 0.5 0.5

1) Amounts expressed as percentage of applied radioact ivity. 2) Area% of HPLC analysis, 14C trace. 3) Area%-mean value of two samples.



### Conclusion: Hydrolysis affects the nature of BYI 08330-keto-hyd roxy residues under conditions being representative for processing studies. At conditions of pH=4 / 90°C (2 0 min) no significant hydrolysis was found. At pH=5 / 100 °C (60 min) ca. 5% degradation was observed. At con ditions of pH=6 / 120 °C (20 min) the test item degraded nearly completely. BYI 08330-MA amide was identified as the hydrolysis product formed.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

B.7.7.1.5 BYI 08330-mono-hydroxy

Reference: BYI 08330-mono-hydroxy: Aqueous hydrolysis under co nditions of processing studies Author(s), year: Koch, Sur; 2006 Report/Doc. number: MEF-05/418 M-267165-01-1 Guideline(s): EU Council Directive 91/414/EEC as am ended by Commission Directive 96/68/EC Section 6.5, Subsection 6.5.1. Guideline 7035/VI/95 Revision 5, Appendix E (July 1997) GLP: Yes. Deviations: None. Validity: The study is considered acceptable.

The purpose of this study was to describe the degra dation behaviour of the BYI 08330-mono-hydroxy in buffered drinking water. The experiments were carri ed out under laboratory conditions which are representative for processing operations of raw agr icultural commodities.

Material and methods: [Azaspirodecenyl-3- 14 

### C]-BYI 08330-mono-hydroxy was applied at a concentr ation of 0.1 mg a.s./L buffer solution. To simulate the conditions of processing studies, non-sterilized drinking water was used. Th e test systems were incubated at three representative sets of hydrolysis conditions:

Pasteurisation: 90 °C at pH 4 for 20 min (water bat h); Baking, brewing, boiling: 100 °C at pH 5 for 60 min (water bath); and Sterilisation: 120 °C at pH 6 for 20 min (autoclave ).

The pH was adjusted to and remained at pH 4, pH 5 a nd pH 6 (each ± 0.2) as required. The temperatures were in the required ranges of 90 ± 3 °C, 100 ± 3 ° C and 120 ± 3 °C during the test periods. The perio ds for heating and cooling to the required temperatures pr ior to and after the incubation, respectively, were not regarded as test periods. The test period started, when the required temperature was reached and was terminated by cooling down, when the test time was over. The 14 

### C-radioactivity of liquid samples was determined by liquid scintillation counting (LSC). Quantitative analysis and identification of the tes t item was performed by TLC- co-chromatography for all samples. Identification of the test item was proven by TLC-co-chromatography with the non-labelled reference item.

Findings: The applied radioactivity was defined as the amount of radioactivity measured in the subsamples taken at the beginning of the incubation period. Based on th e results of LSC measurements immediately after tes t termination, a radioactivity balance was establishe d for each experiment. The material balances ranged from

100.0% to 110.2. The material balances demonstrate that no radioacti vity and no volatile degradation products dissipate d from the test system. The concentration effect is due to the evaporation of water from the test system duri ng processing.

BYI 08330-mono-hydroxy was stable under conditions at pH=4 / 90°C and pH=5 / 100°C as well as under conditions of pH=6 / 120°C. No hydrolysis product w as detectable. Since in none of the samples any hydrolysis product was detectable, no quantitative evaluation of the TLC-analysis was performed. The measured radioactivity in test solutions is pre sented in Table B.7.7.1.5-1.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.7.1.5-1: Measured radioactivity in test s olutions: BYI 08330- mono-hydroxy [0.1 mg/L] time pH

/ temp. Total [Bq] Mean Total

[Bq] samples Test item equivalents [μg/L] 1)

pH=4 90 °C 140.42

141.25 140.8 103.3

pH=5 100 °C 143.75

142.92 143.3 105.2 Zero time

pH=6 120 °C 134.58

143.75 139.2 102.2

pH=4 90 °C 161.25

149.17 155.2 113.9

pH=5 100 °C 146.25

148.33 147.3 108.1 Test termination

pH=6 120 °C 135.00

143.33 139.2 102.1



### Conclusion: BYI 08330-mono-hydroxy remains unaffected under con ditions being representative for processing studies

. Neither at conditions of pH=4 / 90°C (20 min) and p H=5 / 100°C (60 min) nor at conditions of pH=6 / 12 0°C (20 min) the test item was hydrolysed or degraded.

Overall conclusion on the effects on the nature of the residue during processing: The behaviour of BYI 08330 and its four metabolites BYI08330-enol, BYI08330-enol-glucoside, BYI08330- ketohydroxy and BYI08330-monohydroxy in buffer solu tion in three representative sets of hydrolysis conditions was studied:

Pasteurisation: 90 °C at pH 4 for 20 min Baking, brewing, boiling: 100 °C at pH 5 for 60 m in Sterilisation: 120 °C at pH 6 for 20 min

At test termination material balances in all tests were in the range of 100-112% of the applied radioa ctivity indicating that no radioactivity dissipated from th e test system. BYI 08330 was demonstrated to be resistant to hydrolysis under conditions being representative for pasteurization. Under conditions representative for baking, boilin g and brewing 15 % of BYI 08330 degraded to BYI08330-enol. Under conditions of sterilization the active substance was nearly completely hydroly sed to BYI08330-enol. BYI 08330-enol was detected as the o nly hydrolysis product. BYI 08330-enol was shown to be resistant to hydrolysis under all test conditions

. BYI 08330-enol-glucoside was resistant to hydrolysis under conditions representative for pasteurisation

. Under conditions representative for baking, brewing and boiling ca.10 % of the test substance was hydrolysed to BYI 08330-enol. Under conditions of s terilization ca. 40 % of the BYI 08330-enol-glucoside was hydrolysed to the enol metabolite

. BYI 08330-ketohydroxy was demonstrated to be resistant to hydrolysis under conditions of pasteurisation

. Under conditions of baking, brewing and boiling a s light degradation to BYI 08330-MA-amide was found (5%). Under conditions of sterilisation BYI 08330-ketohydroxy was completely hydrolysed to BYI 08330-MAamide

. BYI 08330-monohydroxy was shown to be resistant under all test condition s.

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B.7.7.2 Residue levels - balance studies on set of representative processes

B.7.7.2.1 Residue levels - balance studies on set o f representative processes with relevance

for PMRA (Canada) and USEPA:

B.7.7.2.1.1 Apple processed commodities

Reference: BYI08330 150 OD - Magnitude of the residue on apple processed commodities Author(s), year: Mackie, S. 2006 Report/Doc. number: Report No.: RAFNY014, Edition Number: M-276832-01-1 Guideline(s): PMRA Directive 98-02; DACO 7.4.5/EPA OPPTS 860.1520 GLP: Yes Deviations: No Validity: Yes

Material and methods:

A processing trial was conducted to measure the mag nitude of spirotetramat (BYI 08330) residue in appl es and apple processed commodities following treatment of apples with BYI 08330 150 OD. Three airblast applications were made to apple trees starting when the apples were about 60% of final size (BBCH 76), with a 14-day retreatment interval (RTI). The first app lication was applied at a rate of 0.793 kg a.i./ha (0.706 lb a.i./A). The second and third applications were ap plied at a rate of 0.701 and 0.700 kg ai/ha/applica tion (0.623 and 0.624 lb a.i./A/application), respective ly. All applications were made in spray volumes of 35-70 gallons per acre (GPA). The total seasonal rate wa s 2.195 kg ai/ha (1.954 lb a.i./A). One control an d one treated bulk apple samples were collected at a 7-da y pre-harvest interval (PHI) and hand delivered on the same day to the processing facility. Prior to proc essing, random subsamples of the control and treate d bulk apple samples were collected for analysis, and the remainder of the apple samples were used to generat e the required processed commodities of apple wet pom ace and juice. In addition, samples of washed frui t, peeled fruit, applesauce, and dried fruit were gene rated for use in the dietary risk assessment for spirotetramat. Processing was performed using proc edures which simulated commercial processing practices.

The total residue of spirotetramat and the metaboli tes was quantitated by high-performance liquid chromatography with tandem mass spectrometry (HPLC- MS/MS) method 00857 using isotopically labeled internal standards. Method validation was performe d prior to sample analysis and concurrent recoverie s were performed during sample analysis to demonstrat e acceptable method performance. The individual analyte residues of spirotetramat (parent) and its metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-mono-hydroxy and BYI 08330-enol-glucoside, we re summed to give a total spirotetramat residue in parent equivalents. The limit of quantitation (LOQ ) was 0.010 ppm for each analyte in apple fruit and processed apple commodities.

The maximum interval of frozen storage for apple fr uit and all processed commodities was 34-90 days. Storage stability data indicated that the combined residues of spirotetramat and the associated metabo lites are stable in plant matrices for up to 718 days. S imilarly, storage stability data for orange juice a nd dried prunes indicated that total residues of spirotetram at were stable for at least 147 days. Therefore, t he length of frozen storage of apple commodities would not af fect the magnitude of total spirotetramat residues observed.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Findings :

The total spirotetramat residues were 0.681 ppm in treated apples and were found to concentrate in app le wet pomace (1.9-fold). No concentration (<onefold) of the total spirotetramat residue was found in ap ple juice (0.4-fold), washed fruit (0.6-fold), peeled f ruit (0.2-fold), applesauce (0.1-fold), or dried fr uit (onefold). These factors are less than the maximum concentrati on factor for apples (14-fold for pomace).

Conclusion:

Washing and peeling of apples did not result in con centration of residues, nor did processing of apple s into applesauce, juice or dried fruit. Total spirotetra mat residues did concentrate slightly in apple wet pomace (1.9-fold). These factors are less than the maximu m concentration factor for apples (14-fold for poma ce).

Comments (RMS): None.

B.7.7.2.1.2 Citrus Processed Commodities

Reference: Amended Report BYI08330 150 OD - Magnitude of the R esidue on Citrus Processed Commodities.  Author(s), year: Lenz, C. 2006 Report/Doc. number: Report No.: RAFNY016, Edition Number: M-277028-01-1 Guideline(s): PMRA Directive 98-02; DACO 7.4.5/EPA OPPTS 860.1520 GLP: Yes. Deviations: No. Validity: Yes.

Reference: BYI08330 100 OD - Reduction of the Residue in Grape fruit from Commercial Washing, Waxing, and Packing Procedures. Author(s), year: Krolski, M. E., 2006 Report/Doc. number: Report No.: RAFN042, Edition Number: M-276675-01-1 Guideline(s): PMRA Directive 98-02; DACO 7.4.5/EPA OPPTS 860.1520 GLP: Yes. Deviations: No. Validity: Yes.

Material and methods:

An orange processing trial was conducted to measure the magnitude of residue on oranges and orange processed commodities. Two foliar applications of spirotetramat 150 OD (oil-dispersible) were made to oranges at a rate of 0.756 to 0.783 lb a.i./A/appli cation (0.848 to 0.878 kg a.i./ha/application) with 19 to 21 days between applications and a preharvest interval (PHI) of 1-day. The total amount of spirotetramat applied was 1.54 lb a.i./A (1.726 kg a.i./ha).

A single control and treated bulk sample of oranges were collected at BBCH 83 (fruit ripe for picking has not yet developed variety specific coloration) to BBCH 89 (fruit ripe for consumption) at a 1-day target P HI. Prior to processing, random sub-samples of the control an d treated bulk orange samples were collected for analysis, and the remainder of the orange samples w ere used to generate the required processed commodities of dried pulp, oil, and juice. Process ing was performed using procedures which simulated

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commercial processing practices. The resultant ora nge raw agricultural commodity (RAC) samples and orange processed commodities were analyzed to deter mine total spirotetramat residue. Difficulties in generating the orange oil processed commodity were encountered during processing which resulted in decreased amounts of orange oil sample available fo r analysis.

The total residue of spirotetramat and the metaboli tes was quantitated by high-performance liquid chromatography with tandem mass spectrometry (HPLC- MS/MS) method 00857 using isotopically labeled internal standards. Method validation and concurre nt recoveries were performed to demonstrate accepta ble method performance. The individual analyte residue s of spirotetramat (parent), BYI 08330-enol, BYI 08 330- ketohydroxy, BYI 08330-mono-hydroxy and BYI 08330-e nol-glucoside were summed to give a total spirotetramat residue in parent equivalents. The l imit of quantitation (LOQ) was 0.05 ppm for each an alyte in oranges and the processed commodities of oranges.

A second study conducted on grapefruit was also sub mitted. The study was conducted to evaluate the reduction of spirotetramat residue in grapefruit fo llowing commercial washing and waxing procedures. A single foliar spray application of spirotetramat 10 0 OD was made to grapefruit trees 7 days before fru it harvest at a target rate of 0.314 lb a.i./acre (0.3 52 kg a.i./ha), with the spray adjuvant Dyne-amic a t a rate of 0.25% (v/v). Grapefruit was collected from both th e treated plot and the control plot at a 7-day PHI and the samples were washed and waxed following typical com mercial citrus processing practices. Triplicate samples from the treated plot and a single sample f rom the control plot were collected before and afte r the washing and waxing process.

The total residue of spirotetramat (parent and the metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-mono-hydroxy, and BYI 08330-enol-glucoside) w as quantitated by method 00857 (LC-MS/MS) using isotopically labeled internal standards. The LOQ w as 0.01 ppm for each individual analyte in grapefru it.

Findings :

Concentration (13.5-fold) of the total spirotetrama t residue was observed in the processed commodity o f orange oil. A slight concentration of total BYI 08 830 residues was observed in orange dried pulp (1.3 -fold) and no concentration (0.40-fold) of total spirotetr amat residue was observed in orange juice. These f actors are within the theoretical concentration factors (1 000-fold for citrus oil and 2-fold for juice). The total residues of spirotetramat and the metabolites BYI 08330-enol , - ketohydroxy, -mono-hydroxy, and -enol-glucoside were quantitated and unwashed grapefruit contained average total spirotetramat residues of 0.061 ppm. A processing factor of 0.10-fold was determined from samples collected before and after the washing and waxing process in grapefruit.

The maximum intervals of frozen storage for orange fruit, juice, dried pulp and oil were 169, 44, 23 a nd 12 days, and for grapefruit were 176 days. Storage st ability data indicated that residues of spirotetram at and the associated metabolites are stable for up to 24 months (718 days). Similarly, storage stability da ta indicated that total residues of spirotetramat were stable for at least 5 months (147 days). Since or ange pulp and oil were analyzed within 30 days after their ge neration, storage stability data for these processe d commodities was not required. Therefore, the inter vals of frozen storage for any of the orange or gra pefruit commodities tested here would not have affected the levels of total spirotetramat residues observed.

Conclusion:

Mean total residues of spirotetramat in orange frui t were 0.62 ppm. Processing of oranges into dried pulp and oil resulted in residues concentrating 1.3-fold and 13.5-fold, respectively. No concentration of residues was observed in juice (0.40-fold decrease). These factors conform with the theoretical concentration factors (1000-fold for citrus oil and 2-fold for juice). T otal spirotetramat residues in washed and waxed gra pefruit

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decreased by a factor of 0.10-fold.

Comments (RMS): None.

B.7.7.2.1.3 Grapes Processed Commodities

Reference: BYI08330 150 OD - Magnitude of the Residue in/on Gr apes Processed Commodities Author(s), year: Mosier, D. 2006 Report/Doc. number: Report No.: RAFNY015, Edition Number: M-277287-01-1 Guideline(s): PMRA Directive 98-02; DACO 7.4.5/EPA OPPTS 860.1520 GLP: Yes. Deviations: No. Validity: Yes.

Material and methods:

A grape processing trial was conducted to measure t he magnitude of spirotetramat residues in grapes an d grape processed commodities following treatment of grapes with spirotetramat 150 OD (oil-dispersible). Two airblast applications of spirotetramat 150 OD were made to grapes at a rate of 0.487 - 0.491 lb a.i./A (0.546 – 0.550 kg a.i./ha) with a 28 to 30-day interval and a preharvest interval (PHI) of 5 to 7 days. The to tal seasonal rate was 0.982 lb a.i./A (1.100 kg a.i./ha ) for the treated plots. Spray volumes ranged from 55.87 gallons per acre (GPA) (522.6 L/ha) to 56.54 GPA (5 28.9 L/ha). Each application was made with Dyne-Am ic adjuvant (0.25% v/v) at concentrated spray volume o f 35 to 70 GPA.

A single control and a treated bulk sample of grape s were collected at the fully ripe fruit stage (BBC H 89) (6- day target PHI). Prior to processing, random subsa mples of the control and treated bulk grape samples were collected for analysis, and the remainder of t he grape samples were used to generate the required processed commodities of raisins and juice. Washed grapes and grape jelly processing was performed using procedures which simulated commercial process ing practices.

The total residue of spirotetramat and the metaboli tes was quantitated by high-performance liquid chromatography with tandem mass spectrometry (HPLC- MS/MS) method 00857 using isotopically labeled internal standards. Method validation and concurre nt recoveries were performed to demonstrate accepta ble method performance. Individual analyte residues of spirotetramat, BYI 08330-enol, and BYI 08330- ketohydroxy, BYI 08330-monohydroxy, and BYI 08330-e nol glucoside were summed to give a total spirotetramat residue in parent equivalents. The l imit of quantitation (LOQ) was 0.01 ppm for each an alyte in grapes and the processed commodities of grapes.

Findings :

Following the exaggerated use of spirotetramat 150 OD on grapes and subsequent processing of grapes in to the required commodities, the total spirotetramat r esidue was found to concentrate in raisins (2.61-fo ld). No concentration (<1-fold) of total spirotetramat resi due was observed in grape juice (0.66-fold), jelly (0.28-fold) or washed berries (0.60-fold).

The maximum interval of frozen storage for grapes a nd processed grape commodities was 179 days. Separate storage stability studies indicate that re sidues of spirotetramat and the metabolites BYI 083 30-enol,

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-ketohydroxy, -mono-hydroxy and -enol-Glc are stabl e in raw agricultural commodities for up to 24 mont hs (718 days) and in processed commodities (orange jui ce and prune fruit) for up to 5 months (147 days).

Conclusion: Total spirotetramat residues were shown to concentr ate in raisins (2.61-fold), and decreased in washed grapes (0.60-fold), juice (0.66 fold) and jelly (0. 28-fold). These factors are within the theoretical concentration factors (4.7-fold for raisins and 1.2 -fold for juice).

Comments (RMS): None.

B.7.7.2.1.4 Hop Cone, Green, Processing and Process ed Fractions

Reference: Determination of the Residues of BYI 08330 in/on Ho p Cone, Green, for Processing and the Processed Fractions (Cone, Kiln- Dried; Beer; Hops Draff; Brewer’s Yeast; Brewer’s Malt) after Sprayin g of BYI 08330 (100 OD) in the Field in Northern France and Germany. Author(s), year: Schöning, R., Billian, P., Helfric h, P. 2006 Report/Doc. number: Report No.: RA-3036/04 Edition Number: M-265067-01-2 Guideline(s): PMRA Directive 98-02; DACO 7.4.5/EPA OPPTS 860.1520 GLP: Yes. Deviations: No. Validity: Yes.

Material and methods:

The purpose of the presented study was to determine the transfer of spirotetramat (100 OD, an oildispersible formulation containing 100 g a.i./L) an d its metabolites (BYI 08330-enol, BYI 08330-ketohy droxy, BYI 08330-mono-hydroxy and BYI 08330-enol-Glc) from green hop cones via kiln-dried hop cones into hop processed commodities (beer) and by-products obtain ed during brewing processing (hops draff; brewer’s yeast; brewer’s malt). From each trial, a treated hop cone sample was taken for processing. Green co ne samples were dried until approx. 10% remaining mois ture to produce kiln-dried hop cones samples for processing using simulated commercial procedures.

Method 00857 was used to determine the total residu es of spirotetramat and its metabolites in hop cone s, beer, hop draff, and brewer’s yeast. Adequate meth od-validation data were provided.

Findings:

Total residues of spirotetramat and the metabolites in green cones ranged from 0.66-1.2 ppm. In kiln- dried cones, total residues of spirotetramat ranged from 1.64-4.34 ppm. In all processed commodities tested (beer, brewer’s yeast, brewer’s malt), total residu es of spirotetramat decreased (<1-fold) relative to kiln dried

cones.

The maximum period of frozen storage for hops cones (green and dried) was 352-358 days, which was within the demonstrated period of storage stability for total spirotetramat residues (18 months). The maximum period of frozen storage for hops draff, br ewer’s yeast, brewer’s malt and beer was 105, 74, 9 5 and 67 days, respectively, also within the demonstr ated period of storage stability for total spirotet ramat residues.

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Conclusion: All processed fractions of hops showed a decrease i n the total spirotetramat residues relative to-kiln dried

cones.

Comments (RMS): None.

B.7.7.2.1.5 Plum Processed Commodities

Reference: BYI 08330 150 OD: Magnitude of the Residue on Plum Processed Commodities Author(s), year: Mackie, S. 2006 Report/Doc. number: Report No.: RAFNY018, Edition Number: M-276380-01-1 Guideline(s): PMRA Directive 98-02; DACO 7.4.5/EPA OPPTS 860.1520 GLP: Yes. Deviations: No. Validity: Yes.

Material and methods:

A plum processing trial was conducted to measure th e magnitude of total spirotetramat residues in plum s and plum processed commodities following treatment of plums with BYI 08330 150 OD (oil-dispersible). Three airblast applications were made to plum trees . The first application was made when the plums we re at the beginning of fruit colouring stage, with a 14-d ay interval between the two succeeding applications . The first application was made at a rate of 0.704 lb a. i./A/application (790 g a.i./ha/application). The second and third test substance applications were made at a ta rget rate of 0.492 lb a.i./A/application (551 g a.i./ha/application) in target spray volumes of 35- 70 gallons per acre (GPA). The achieved total seas onal rate was 1.69 lb a.i./A (1892 g a.i./ha).

One control and one treated bulk plum samples were collected at a 7-day pre-harvest interval (PHI) and shipped on the same day to the processing facility. Prior to processing, random sub-samples of the co ntrol and treated bulk plum samples were collected for an alysis, and the remainder of the plum samples was u sed to generate the required processed commodities of p runes. In addition, samples of washed plum fruit w ere generated.

The total residue of spirotetramat and the metaboli tes was quantitated by high-performance liquid chromatography with tandem mass spectrometry (HPLC- MS/MS) method 00857 using isotopically labeled internal standards. Method validation was performe d prior to sample analysis and concurrent recoverie s were performed during sample analysis to demonstrat e acceptable method performance. The individual analyte residues of spirotetramat (parent) and the metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-mono-hydroxy and BYI 08330-enol-glucoside, we re summed to give a total spirotetramat residue in parent equivalents. The limit of quantitation (LOQ ) was 0.01 ppm for each analyte in the plum raw agricultural commodity (RAC) and each processed com modity.

Findings :

The maximum interval of frozen storage for plum fru it and all processed commodities ranged from 84 day s to 140 days. Storage stability data indicated that th e combined residues of spirotetramat and the associ ated metabolites are stable in plant matrices for up to 24months (718 days). Similarly, storage stability data for orange juice and dried prunes indicated that total residues of spirotetramat were stable for at least 5 months

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(147days).

The total spirotetramat residue was found to concen trate in prunes (2.2-fold). No concentration (<1-f old) of total spirotetramat residue was found in washed plu m fruit (0.9-fold).

Conclusion: Plums washed and processed into prunes had processi ng factors of 0.9-fold and 2.2-fold, respectively. These factors were within the theoretical concentra tion factor (3.4-fold for prunes).

Comments (RMS): None.

B.7.7.2.1.6 Potato Processed Commodities

Reference: BYI 08330 150OD - Magnitude of the Residue on Potat o Processed Commodities. Author(s), year: Lenz, C. 2006 Report/Doc. number: Report No.: RAFNY020, Edition Number: M-276828-01-1 Guideline(s): PMRA Directive 98-02; DACO 7.4.5/EPA OPPTS 860.1520 GLP: Yes. Deviations: No. Validity: Yes.

Material and methods:

A potato processing trial was conducted to measure the magnitude of spirotetramat residue on potatoes and potato processed commodities. Two foliar applicati ons of spirotetramat 150 OD (oil-dispersible) were made to potatoes at a rate of ~0.450 kg a.i./ha (0.40 lb s. a.i./A) with 7 days between applications. A sin gle control and a treated bulk sample of potatoes were collecte d at a 7-day pre-harvest interval (PHI). Prior to processing, random sub-samples of the control and t reated bulk potato samples were collected for analy sis, and the remainder of the potato samples were used t o generate the required processed commodities of we t peel, chips, and granules.

In addition, samples of washed potatoes, cooked pot atoes, and potato tuber without peel were generated for use in the dietary risk assessment for spirotetrama t. Potato processing was performed using procedure s which simulated commercial processing practices. T he resultant potato samples and processed commodities were analyzed to determine total residu es of spirotetramat and its metabolites. The potat o tuber raw agricultural commodity (RAC) and processe d commodities were held in frozen storage for a maximum of <1 month (8-13 days) prior to analysis. Storage stability data for the processed commoditi es are thus not required.

The total residue of spirotetramat and the metaboli tes was quantitated by high-performance liquid chromatography with tandem mass spectrometry (HPLC- MS/MS) method 00857 using isotopically labeled internal standards. Method validation and concurre nt recoveries were performed to demonstrate accepta ble method performance. The individual analyte residue s of spirotetramat (parent), BYI 08330-enol, BYI 08 330- ketohydroxy, BYI 08330-mono-hydroxy and BYI 08330-e nol-glucoside were summed to give a total spirotetramat residue in parent equivalents. The l imit of quantitation (LOQ) was 0.01 ppm for each an alyte in potatoes and the processed commodities of potatoes.

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Findings:

The maximum concentration of total spirotetramat re sidues was observed in processed potato flakes (3.5

- fold). A slight concentration of total spirotetram at residue was observed in potato chips (1.2-fold) and no concentration of total spirotetramat residue was ob served in potato wet peel (1-fold).

Conclusion: The processing factors observed are within the theo retical concentration factors (4.7-fold for flakes and 4-fold for processed waste).

Comments (RMS): None.

B.7.7.2.1.7 Tomato Processed Commodities

Reference: BYI08330 100 OD - Magnitude of the residue on tomat o processed commodities Author(s), year: Mackie, S. J. W. 2006 Report/Doc. number: Report No.: RAFNY013, Edition Number: M-277034-01-1 Guideline(s): PMRA Directive 98-02; DACO 7.4.5/EPA OPPTS 860.1520 GLP: Yes. Deviations: No. Validity: Yes.

Material and methods:

A tomato processing trial was conducted to measure the magnitude of spirotetramat (BYI 08330) residue in tomatoes and tomato processed commodities. Two bro adcast foliar applications of BYI 08330 100 OD (oil

dispersion containing 100 g/L or 0.83 lb/gallon spi rotetramat) were made to tomato plants. The first application was made when 20% of the tomatoes showe d typical full ripe colour (BBCH 82), with a 7-day interval between the two applications. The two app lications were applied at a rate of 0.397-0.440 lb a.i./A/application (0.445-0.449 kg a.i./ha/applicat ion). One control and one treated bulk tomato samp le were collected at a 3-day pre-harvest interval (PHI). P rior to processing, random sub samples of the contr ol and treated bulk tomato samples were collected for anal ysis, and the remainder of the tomato samples were used to generate the required processed commodities of purée, paste, and juice. In addition, samples of washed tomatoes, cooked (hot crushed) tomatoes, can ned tomatoes, and dried tomatoes were generated.

The total residue of spirotetramat and the metaboli tes was quantitated by high-performance liquid chromatography with tandem mass spectrometry (HPLC- MS/MS) method 00857 using isotopically labelled internal standards. Method validation was performe d prior to sample analysis and concurrent recoverie s were performed during sample analysis to demonstrat e acceptable method performance. The individual analyte residues of spirotetramat (parent) and the metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-mono-hydroxy and BYI 08330-enol-glucoside, we re summed to give a total spirotetramat residue in parent equivalents. The limit of quantitation (LOQ) was 0.01 ppm for each analyte in the tomato raw agricultural commodity (RAC) and each processed com modity.

Findings :

The total spirotetramat residue was found to concen trate in dried tomatoes (12-fold), tomato paste (7. 4-fold) and in tomato purée (3.5-fold). No concentration ( <1-fold) of the total spirotetramat residue was fou nd in

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tomato juice (0.9-fold). In the addition, the tota l spirotetramat residue was found to concentrate in canned tomatoes (1.1-fold) and dried tomatoes (12-fold). No concentration ( ≤ 1-fold) of total spirotetramat residue was found in the washed tomatoes (0.7-fold), or coo ked (hot crushed) tomatoes (0.6-fold).

Conclusion:

The processing factors observed in some cases exce ed the theoretical concentration factors for tomato (1.4- fold for purée, 1.4-fold for juice, and 5.5-fold fo r paste).

Comments (RMS): None.

Overall conclusion :

Acceptable apple, orange, grape, plum, potato, hop and tomato processing studies are available. The processing studies show that following processing o f RAC samples bearing quantifiable residues, total residues of spirotetramat and the metabolites conce ntrated in apple wet pomace (1.9-fold), citrus oil (13.5- fold), orange dried pulp (1.3-fold), raisins (2.6-f old), prunes (2.2-fold), potato flakes (3.5-fold), potato chips (1.2-fold), dried tomatoes (12-fold), tomato paste (7.4-fold) and tomato purée (3.5-fold). MRLs will o nly be necessary for potato flakes, raisins, and citrus oi l.

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B.7.7.2.2 Residue levels - balance studies on set o f representative processes with relevance

for the European Community (EU)

B.7.7.2.2.1 Orange juice and marmalade

Reference: Determination of the residues of BYI 08330 in/on or ange fruit and the processed fractions (pulp, peel, raw juice; pomace wet, washings, fruit washed, marmalade, peelwashed, fruit peeled, strain rest, peel dried, pomace dried) after spraying of BYI 08330 (100 OD) in the field in Italy, Portugal and Spain Author(s), year: Schoening R., Helfrich P.; 2006 Report/Doc. number: RA-3032/04, including samples f rom trials no. R 2004 0139/6, R 2004 0141/8, R 2004 0239/2, R 2004 0240/6 M-263630-01-1 Guideline(s): EU Council Directive 91/414/EEC of Ju ly15, 1991, Annex II, part A, section 6 and Annex III, part A, section 8: Residues in or on tr eated products, food and feed GLP: Yes. Deviations: None. Validity: The study is considered acceptable. The purpose of the presented study was to determine the transfer of BYI 08330 and its metabolites (BYI08330-enol, BYI08330-ketohydroxy, BYI08330-mono -hydroxy and BYI08330-enol-Glc) from orange fruit into processed fractions after processing of orange fruits to juice and marmalade.

Material and methods: Orange fruit samples from four field trials that we re performed in Italy, Portugal and Spain as part o f study RA-2032/04 with BYI 08330 (100 OD) were processed. From each of the 4 trials two fruit samples (one fo r juice processing and one for marmalade processing) have been taken. Information about the treated plot s is given in Table B.7.7.2.2.1-1.

Table B.7.7.2.2.1-1: Application Data Summary in/o n Orange in Southern Europe.

Country Trial No. Number Formulation Kg a.s./ha Kg a.s./ha x m *) Growth stage

BBCH Italy R 2004 0139/6 2 OD 100 0.2112 0.096 87

Italy R 2004 0141/8 2 OD 100 0.2300 0.096 85-88

Portugal R 2004 0239/2 2 OD 100 0.2880 0.096 81-83

Spain R 2004 0240/6 2 OD 100 0.2880 0.096 79-81

*) Rate per m height of leafy surface



### Preparation of processed fractions: The oranges were processed simulating industrial pr ocedures, whereby the degradation of the active ingredients was kept to a minimum (worst case situa tion). This was achieved by a minimum of processing steps. Basis of the juice processing was the squeez ing of orange halves by means of an electrical juic e squeezer. The marmalade was produced by cooking the orange pulp and cut orange peel with jam sugar.

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Table B.7.7.2.2.1-2: Preparation of orange (RAC) t o processed fractions:

Production of orange juice Production of orange marma lade Defrosting : The orange specimens were defrosted at room temperature. Defrosting : The orange specimens were defrosted at room temperature. Washing : The oranges were cleaned in two steps with tap wate r. The washed oranges were used for the preparation of juice and of additional products. An aliquot of washed fruit and washings (washing water) was taken as a specimen. Washing : The oranges were cleaned in two steps with tap wate r. The washed oranges were used for the preparation of the marmalade.

Extraction of the juice : A portion of the washed oranges was cut into halves and squeezed using a citrus juice squeezer. The peel wi th rest of the endocarp remaining after squeezing gave the fraction peel, washed. Pomace (seeds and the orange flesh) was separated by sieving the juice through a colander. The pomace was centrifuged (= pomace, wet ). The supernatant juice was combined with the squeeze d juice to the raw juice. A portion of the pomace, wet and a portion of the peel, washed was dried in the range of 40 to 80°C1 until the water content is close to 10 %. An aliquot of the following fractions was taken as a specimen: raw juice

, washed peel

, dried peel ; wet pomace , and dried pomace

. Peeling of the oranges : The oranges were manually peeled. Approx. 3.8 – 5.3 kg of peeled fruit and 1.7 to 2.4 kg of peel were prod uced. The peel was cut into strips. An aliquot of peeled fruit and washed peel were taken as specimens.

Homogenisation of the oranges: The peeled oranges were cut into pieces. The pieces were homogenised using a food processor (cutter).The homogenised oranges were heated to approx. 100°C. T he heated homogenate was sieved through a colander at a temperature range of 57 to 81°C. The orange pulp wi thout seed and crude parts of the fruit was used for the preparation of the marmalade. An aliquot of the rema ining on the colander ( strain rest ) was taken as a specimen. Pasteurisation : The raw juice was transferred into glass bottles (1 L) and tightly closed. The bottles were heated within 45 t o 60 min from 27 – 31°C to approx. 80°C. After 15 min at 82 t o 86°C (final temperature) they were cooled down to r oom temperature over night. An aliquot of the juice (pasteurised) was taken as a specimen.

Preparation of the marmalade : The marmalade consisted of 65 % jam sugar, 10 % pee l and 25 % orange pulp (e.g. 4875 g of sugar were combined with 750 g of peel and 1875 g of orange pu lp). The mixture was heated in a cooking pot under stirr ing. The marmalade was cooked for a few minutes (10 – 15 min.). At the end the marmalade was transferred into jam jars and cooled down to room temperature over night

. An aliquot of the marmalade was taken as a specimen.



### Residues of BYI 08330 and its metabolites BYI08330- enol, BYI08330-ketohydroxy, BYI08330-mono-hydroxy and BYI08330-enol-Glc in/on orange (fruit; raw juic e; juice; pomace, wet; washings; fruit, washed; pom ace, dried; peel, dried; peel, washed; marmalade; fruit, peeled; strain rest) were determined by HPLC-ESIMS/MS. The Limit of Quantitation (LOQ), defined as the lowest validated fortification leve l (calculated as BYI 08330 equivalents), was 0.01 mg/kg (BYI 08330), 0.012 mg/ kg (BYI08330-enol, BYI08330-ketohydroxy, BYI08330- mono-hydroxy) and 0.008 mg/kg (BYI08330-enol-Glc) i n/on orange (fruit; raw juice; juice; pomace, wet; washings; fruit, washed; pomace, dried; peel, dried ; peel, washed; marmalade; fruit, peeled; strain re st). The LOQ for the total residue of BYI 08330 (sum of sing le analyte residues, each calculated as BYI 08330 equivalents) was calculated as 0.054 mg/kg in/on or ange (fruit; raw juice; juice; pomace, wet; washing s; fruit, washed; pomace, dried; peel, dried; peel, washed; m armalade; fruit, peeled; strain rest).

Procedural recoveries: Recovery findings in the different processed matric es were within guideline requirements (70-110%, RSD <20%). Recovery results are summarized in Table B.7 .7.2.2.1-3.

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Table B.7.7.2.2.1-3: Recovery results (concurrent recoveries) for determination of BYI 08330 and its metabolites in orange fruit and in processed commod ities Sample Material Orange Fruit 1) Orange Peel 2) Orange Juice 3) Orange Wet Pomace 4) Orange

Marmalade

Analyte Fortification levels *) Mean

Recovery [%±RDS] Fortification levels Mean

Recovery [%±RDS] Fortification levels Mean

Recovery [%±RDS] Fortification levels Mean

Recovery [%±RDS] Fortification levels Mean

Recovery [%±RDS]

BYI 08330 0.01

1.0 88 ±

13.0 (n=15) 0.01

002 1.0 83 ±

12.5 (n=16) 0.01

1.0 83 ±

9.8 (n=8) 0.01

1.0 81 ±

9.8 (n=8) 0.01

1.0 90 ±

5.7 (n=8)

BYI08330- enol 0.01

1.0 86 ±

9.9 (n=15) 0.01

002 1.0 82 ±

11.9 (n=16) 0.01

1.0 83 ±

10.0 (n=8) 0.01

1.0 82 ±

12.5 (n=8) 0.01

1.0 90 ±

4.9 (n=8)

BYI08330- ketohydro xy 0.01

1.0 85 ±

9.1 (n=8) 0.01

002 1.0 82 ±

12.1 (n=8) 0.01

1.0 83 ±

12.4 (n=8) 0.01

1.0 81 ±

11.4 (n=8) 0.01

1.0 88 ±

6.1 (n=8)

BYI08330-

monohydroxy 0.01

1.0 85 ±

10.3 (n=15) 0.01

002 1.0 83 ±

12.1 (n=16) 0.01

1.0 81 ±

9.6 (n=8) 0.01

1.0 80 ±

12.9 (n=8) 0.01

1.0 88 ±

7.0 (n=8)

BYI08330- enol-Glc 0.01

1.0 86 ±

9.9 (n=15) 0.01

002 1.0 83 ±

11.0 (n=16) 0.01

1.0 79 ±

13.5 (n=8) 0.01

1.0 83 ±

11.3 (n=8) 0.01

1.0 90 ±

7.2 (n=8)

1) Sample material fruit covers sample materials pulp ; fruit, washed; fruit, peeled.

2) Sample material peel covers sample materials peel, dried; peel, washed.

3) Sample material juice covers sample materials raw juice; washings.

4) Sample material pomace, wet covers sample material s pomace, dried; strain rest. *) levels refer to fortification with individual anal ytes (not calculated as BYI 08330 equivalents).



### Findings: The total residue of BYI08330 in orange fruit used for processing ranged between <0.054 mg/kg (LOQ) an d 0.18 mg/kg. In orange juice from all 4 orange fruit samples a total residue of below the LOQ of 0.054 mg/kg was detected. In orange marmalade the total residue of BYI 08330 ranged between <0.054 and 0.067 mg/kg. The residue results for the different proces sed fractions are given in Table B.7.7.2.2.1-4 and Table B.7.7.2.2.1-5.

Table B.7.7.2.2.1-4: Residues of BYI 08330 in oran ge fruit and in processed commodities from orange juice processing Residues [mg/kg] Country / Trial No. Portion

analysed PHI

[days] BYI 08330 BYI 08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total Res.

of BYI 08330 calc. Italy R 2004 0139/6 fruit

raw juice juice pomace, wet washings fruit, washed pomace, dried peel, dried peel, washed 14 0.02

0.01 <0.01 <0.01 0.01 0.01 0.01 0.02 0.02 0.012

<0.012 <0.012 <0.012 <0.012 0.012 0.014 0.16 0.018 0.012

0.012 <0.012 <0.012 0.012 0.012 0.013 0.097 0.019 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.008 <0.054

<0.054 <0.054 <0.054 <0.054 <0.054 <0.054 0.27 0.057

### - 161 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues [mg/kg] Country / Trial No. Portion

analysed PHI

[days] BYI 08330 BYI 08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total Res.

of BYI 08330 calc. Italy R 2004 0141/8 fruit

raw juice juice pomace, wet washings fruit, washed pomace, dried peel, dried peel, washed 21 0.02

<0.01 <0.01 <0.01 <0.01 0.01 <0.01 0.03 0.01 0.014

<0.012 <0.012 <0.012 <0.012 0.013 0.016 0.094 0.024 0.012

<0.012 <0.012 <0.012 <0.012 0.012 0.012 0.042 0.013 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.008 <0.008 0.012 0.008 <0.054

<0.054 <0.054 <0.054 <0.054 <0.054 <0.054 0.18 0.059 Portugal R 2004 0239/2 fruit

raw juice juice pomace, wet washings fruit, washed pomace, dried peel, dried peel, washed 14 0.04

<0.01 <0.01 <0.01 <0.01 0.02 0.01 0.07 0.03 0.041

<0.012 <0.012 <0.012 <0.012 0.036 0.041 0.26 0.059 0.012

<0.012 <0.012 <0.012 <0.012 0.013 0.012 0.083 0.024 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.008

<0.008 <0.008 <0.008 <0.008 0.008 <0.008 0.018 0.008 0.099

<0.054 <0.054 <0.054 <0.054 0.073 0.062 0.43 0.12 Spain R 2004 0240/6 fruit

raw juice juice pomace, wet washings fruit, washed pomace, dried peel, dried peel, washed 21 0.08

0.01 0.01 0.01 0.02 0.04 0.01 0.15 0.06 0.078

0.030 0.026 0.041 0.012 0.062 0.22 0.36 0.073 0.012

<0.012 <0.012 <0.012 <0.012 0.012 0.012 0.064 0.016 <0.012

<0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 <0.012 0.016

0.008 0.008 0.008 <0.008 0.017 0.019 0.063 0.020 0.18

<0.054 <0.054 0.059 <0.054 0.13 0.26 0.64 0.17



### Table B.7.7.2.2.1-5: Residues of BYI 08330 in orang e fruit and in processed commodities from orange marmalade processing Residues [mg/kg] Country / Trial No. Portion

analysed PHI

[days] BYI 08330 BYI 08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total Res.

of BYI 08330 calc. Italy R 2004 0139/6 fruit

peel, washed marmalade fruit, peeled strain rest 14 0.02

0.06 <0.01 <0.01 <0.01 0.012

0.030 <0.012 <0.012 <0.012 0.012

0.034 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.008

<0.008 <0.008 <0.008 <0.008 <0.054

0.12 <0.054 <0.054 <0.054 Italy R 2004 0141/8 fruit

peel, washed marmalade fruit, peeled strain rest 21 0.02

0.02 <0.01 <0.01 <0.01 0.014

0.027 <0.012 <0.012 <0.012 0.012

0.013 <0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 <0.008

0.008 <0.008 <0.008 <0.008 <0.054

0.067 <0.054 <0.054 <0.054 Portugal R 2004 0239/2 fruit

peel, washed marmalade fruit, peeled strain rest 14 0.04

0.04 0.01 <0.01 <0.01 0.041

0.080 0.013 <0.012 <0.012 0.012

0.031 0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 0.008

0.008 <0.008 <0.008 <0.008 0.099

0.16 <0.054 <0.054 <0.054

### - 162 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues [mg/kg] Country / Trial No. Portion

analysed PHI

[days] BYI 08330 BYI 08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total Res.

of BYI 08330 calc. Spain R 2004 0240/6 fruit

peel, washed marmalade fruit, peeled strain rest 21 0.08

0.14 0.01 0.01 0.01 0.078

0.11 0.036 0.064 0.054 0.012

0.034 0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012 0.016

0.046 0.008 0.010 0.008 0.18

0.33 0.067 0.084 0.072



### Based on the residue levels in the treated processi ng products transfer factors were calculated. The t ransfer factors for the processing products are calculated according to the following equation:

Transfer Factor = Residue concentration in the proc essed product [mg/kg] / Residue concentration in th e RAC [mg/kg]

Transfer factors are calculated on a worst-case bas is. For this purpose, residues < LOQ are set at the LOQ. A mean average factor of 0.5 was calculated for the transfer of the total residue of BYI08330 from ora nge fruit into orange juice and orange marmalade. The t ransfer factors are summarized in Table B.7.8.1.1-6 . No transfer factors could be calculated for processed commodities from two trials (R 2004 0139/6 and R 20 04 0141/8), because the total residue of BYI08330 in o range fruit and in processed commodities was below the LOQ.

Table B.7.7.2.2.1-6: Transfer factors for the tota l residue of BYI08330 into processed commodities related to orange fruit

Transfer Factors for Total Residue of BYI08330

Sample material R 2004 0239/2 R 2004 0240/6 mean

washings 0.6 0.3 0.5 fruit, washed 0.7 0.7 0.7 raw juice 0.6 0.3 0.5 peel, washed 1.2 0.9 1.1 peel, dried 4.3 3.6 4.0 pomace, wet 0.6 0.3 0.5 pomace, dried 0.6 1.4 1.0 Orange juice

juice 0.6 0.3 0.5 peel, washed 1.6 1.8 1.7 fruit, peeled 0.6 0.5 0.6

strain rest 0.6 0.4 0.5 Orange marmalade

marmalade 0.6 0.4 0.5



### Conclusion : As an average factor of 0.5 could be calculated for the transfer of the total residue of BYI08330 from orange fruit into orange juice and orange marmalade, no co ncentration of BYI08330 is to be expected during processing of oranges to juice and marmalade. Conce ntration was observed in peel; however, these resul ts are not meaningful, as under household conditions o range peel will not be consumed as edible portion per

se . Under industrial juice processing conditions the fruits are processed unpeeled; this process was not simulated in the present study. No concentration in wet pomace (possible feed item) was observed.

### - 163 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

B.7.7.2.2.2 Apple sauce and juice

Reference: Determination of the residues of BYI 08330 in/on ap ple fruit and the processed fractions (fruit washed, washings, strain rest, raw sauce, sauce, raw juice, juice, pomace dried) after spraying of B YI 08330 (100 OD) in the field in Germany and United Kingdom Author(s), year: Schoening R., Helfrich P.; 2005, a mended 12.01.2006 Report/Doc. number: RA-3135/04, including trials no . R 2004 0795/5, R 2004 0797/1 M-262624-02-1 Guideline(s): EU Council Directive 91/414/EEC of Ju ly15, 1991, Annex II, part A, section 6 and Annex III, part A, section 8: Residues in or on treated products, food and feed GLP: Yes. Deviations: None. Validity: The study is considered acceptable.

Reference: Determination of the residues of BYI 08330 in/on ap ple fruit and the processed fractions (fruit washed, washings, strain rest, raw sauce, sauce, raw juice, juice, pomace dried) after spraying of B YI 08330 (100 OD) in the field in Italy and Spain Author(s), year: Schoening R., Helfrich P.; 2006 Report/Doc. number: RA-3137/04, including trials no . R 2004 0805/6, R 2004 0807/2 M-264335-01-1 Guideline(s): EU Council Directive 91/414/EEC of Ju ly15, 1991, Annex II, part A, section 6 and Annex III, part A, section 8: Residues in or on treated products, food and feed GLP: Yes. Deviations: None. Validity: The study is considered acceptable.

The purpose of the presented studies was to determi ne the transfer of BYI 08330 and its metabolites (BYI08330-enol, BYI08330-ketohydroxy, BYI08330-mono -hydroxy and BYI08330-enol-Glc) from apple fruits into processed fractions fruit, washed; washings (w ashing water); strain rest (pomace, wet); raw sauce (raw stewed fruit); sauce; raw juice; juice; pomace, dri ed.

Material and methods: Apple fruit samples from four field trials that wer e performed in Germany, United Kingdom, Italy and S pain as part of study RA-2135/04 and study RA-2137/04 were processed. For each process, washing, sauce and juice production, 4 representative samples of apple fruits from each those 4 supervised residue trials were used. Information about the treated plots is given in Table B.7.7.2.2.2-2.

Table B.7.7.2.2.2-1: Application Data Summary in/o n Apples in Northern and Southern Europe.

Country Trial No. Number Formulation Kg a.s./ha Kg a.s./ha x m *) Growth stage

BBCH Germany R 2004 0795/5 2 OD 100 0.144 0.072 76-77

United Kingdom R 2004 0797/1 2 OD 100 0.137 0.072 85

Italy R 2004 0805/6 2 OD 100 0.216 0.072 79-81

### - 164 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Country Trial No. Number Formulation Kg a.s./ha Kg a.s./ha x m *) Growth stage

BBCH Spain R 2004 0807/2 2 OD 100 0.216 0.072 77-81

*) Rate per m height of leafy surface



### Preparation of processed fractions: The apples were processed into washed fruit, washin g water (washings), strain rest (pomace wet), raw sauce (raw stewed fruit), sauce, raw juice, juice a nd pomace dried simulating household and industrial procedures (see Table B.7.7.2.2.2-2). The washing s imulated household processing, whereas the apple sauce and juice processing simulated the industrial practice at a laboratory scale.

Table B.7.7.2.2.2-2: Preparation of apple (RAC) to processed fractions:

Processing of Apple Fruit into Washed Fruit and Washing Water Processing of Apple Fruit into Strain rest (pomace wet), Raw

Stewed Fruit and Wet Pomace Processing of Apple Fruit into Pomace Dried, Raw Juice and

Juice

Damaged apples were sorted out. Stalks and leaves we re removed. Then the apple fruits were washed for 1 to 2 min. in lukewarm standing water (ratio water/fruits = 2/1 ( w/w)) by moving them around slowly. After washing, t he apples were let to drain in a sieve. The laboratory sample of fruit, washed was prepared by cutting the apples in four parts and filling them into a plastic bag. The laboratory sample of washing water was prepared by filling a portion of the washing water in polystyrene boxes. The washed fruits were cut in four or eight pieces using a knife. For blanching, the apple pieces were heated to 98 – 100°C; the blanching time depends on the degree of ripeness. After the blanching process was finished, the apple pulp was passed through a strainer in order to separate raw stewed fruit and wet pomace (strain rest ). The remaining raw stewed fruit was weighed, mixed up with sugar (w (sugar) = 16.5 %) and filled into 1/1 preserving cans. The preserving cans were pasteurised in an autoclave. After pasteurisation, the preserving cans were emptied in a larger vessel, mixed thoroughly and weighed. The washed apples were crushed into mash in a cutter. The obtained mash was pressed in a high-pressure press into raw juice and wet pomace. The wet pomace was dried in a fanassisted oven at about 100°C until the water content was nearly 10 %. The remaining raw juice was enzymated by heating the juice in a cooking pan for about 0.5 to 2 minutes at 80 – 90°C. After cooling down to 45 – 50°C, pectolytic enzymes were added and the juice was left to stand for one hour at room temperature. The juice was stored for approx. 20 hours (overnight) at 4°C. Afterwards, the juice was fined coarsely by lifting up it by a tube andcentrifugation of the lees. The Brixvalues of the filtrate and the retentate were determined. The coarsely finedjuice was filtrated in a laboratory ultrafiltration set-up into the clear juice. Thereupon, the filtrated juice waspasteurised in a plate heatexchanger. After pasteurisation, the juice was collected in fractions. Onlythe fractions that had the same Brixvalue as the filtrate were collected in a bigger container and constituted the sample pasteurised juice

.



### Residues of BYI 08330 and its metabolites BYI08330- enol, BYI08330-ketohydroxy, BYI08330-mono-hydroxy and BYI08330-enol-Glc in/on apple (fruit) were dete rmined by HPLC-ESI-MS/MS. The Limit of Quantitation (LOQ), defined as the lowest validated fortification leve l (calculated as BYI 08330 equivalents), was 0.01 mg/kg (BYI 08330), 0.012 mg/ kg (BYI08330-enol, BYI08330-ketohydroxy, BYI08330- mono-hydroxy) and 0.008 mg/kg (BYI08330-enol-Glc) i n/on apple (fruit). The LOQ for the total residue o f BYI 08330 (sum of single analyte residues, each calcula ted as BYI 08330 equivalents) was calculated as 0.0 54 mg/kg in/on apple (fruit).

### - 165 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Recovery results are summarized in Table B.7.7.2.2.2-3.

Table B.7.7.2.2.2-3: Recovery results (concurrent recoveries) for BYI 08330 and its metabolites in apple fruit and processed commodities (Report No.: 3135/04, amended, including trials No. R 2004 0795/5 and R 2004 0797/1; Report No.: 3137/04 inclu ding trials No. R 2004 0805/6 and R 2004 0807/2) Sample Material Apple fruit 1) Strain rest 2) Apple sauce 3)

Analyte Forti-fication levels *) Mean Recovery

[%±RDS] Forti-fication levels Mean Recovery

[%±RDS] Forti-fication levels Mean Recovery

[%±RDS]

BYI 08330 0.01

1.0 97 ± 8.1

(n=27) 0.01

1.0 102 ± 8.1

(n=6) 0.01

1.0 94 ± 11.6

(n=6)

BYI08330-enol 0.01

1.0 92 ± 7.0

(n=27) 0.01

1.0 98 ± 3.7

(n=6) 0.01

1.0 90 ± 7.8

(n=6)

BYI08330- ketohydroxy 0.01

1.0 97 ± 7.6

(n=27) 0.01

1.0 103 ± 6.9

(n=6) 0.01

1.0 97 ± 10.9

(n=6)

BYI08330-monohydroxy 0.01

1.0 92 ± 7.2

(n=27) 0.01

1.0 98 ± 3.6

(n=6) 0.01

1.0 93 ± 6.4

(n=6)

BYI08330-enol-Glc 0.01

1.0 96 ± 8.3

(n=27) 0.01

1.0 107 ± 8.6

(n=6) 0.01

1.0 100 ± 7.7

(n=6)

1) Fruit covers fruit, washed; raw juice; juice and w ashings.

2) Strain rest covers pomace, dried.

3) Sauce covers raw sauce. *) levels refer to fortification with individual anal ytes (not calculated as BYI 08330 equivalents). 

### The mean of the recoveries were for all matrices an d for all fortification levels, within the acceptab le range of

70 – 110 %.

Findings : The total residue of BYI08330 in apple fruit was be tween <0.054 (LOQ) and 0.2 mg/kg. In apple sauce, t he total residue ranged between <0.054 and 0.13 mg/kg and was between <0.054 and 0.078 mg/kg in apple juice. Average factors of 0.6 and 0.8 were calculat ed for the transfer of the total residue of BYI0833 0 from apple fruit into apple juice and apple sauce. The r esidues results are summarised in Table B.7.7.2.2.2 -4. Transfer factors are given in Table B.7.7.2.2.2-5.

Table B.7.7.2.2.2-4: Residues of BYI 08330 in appl e fruit and in processed commodities Residues [mg/kg] Country / Trial No. Portion

analysed PHI

[days] BYI 08330 BYI 08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total Res.

of BYI 08330 calc. Germany R 2004 0795/5 fruit

fruit, washed washings

APPLE SAUCE : strain rest

raw sauce

sauce APPLE JUICE : raw juice juice pomace, dried 21 0.01 0.02 <0.01

0.05 0.01 0.01

<0.01 <0.01 0.16 0.012

0.012 <0.012

0.029 0.018 0.016

0.012 0.012 0.092 0.012

0.016 <0.012

0.025 0.017 0.013

0.012 0.012 0.077 0.012

0.012 <0.012

0.012 0.012 0.012

0.012 0.012 0.013 <0.008

0.008 <0.008

0.008 0.008 <0.008

0.008 0.008 0.008 <0.054

0.064 <0.054

0.13 0.066 <0.054

<0.054 <0.054 0.35

### - 166 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues [mg/kg] Country / Trial No. Portion

analysed PHI

[days] BYI 08330 BYI 08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total Res.

of BYI 08330 calc.

United Kingdom R 2004 0797/1 fruit

fruit, washed washings

APPLE SAUCE : strain rest

raw sauce

sauce APPLE JUICE : raw juice juice pomace, dried 21 0.04 0.02 <0.01

0.12 0.03 0.02

0.02 0.01 0.31 0.034

0.020 <0.012

0.055 0.044 0.039

0.024 0.019 0.22 0.021

0.012 <0.012

0.026 0.021 0.017

0.016 0.013 0.094 <0.012

<0.012 <0.012

<0.012 <0.012 <0.012

<0.012 <0.012 0.012 <0.008

<0.008 <0.008

<0.008 <0.008 <0.008

<0.008 <0.008 0.008 0.096

<0.054 <0.054

0.20 0.098 0.075

0.058 <0.054 0.65 Italy R 2004 0808/6 fruit

fruit, washed washings

APPLE SAUCE : strain rest

raw sauce

sauce APPLE JUICE : raw juice juice pomace, dried 21 0.04 0.02 <0.01

0.06 0.01 0.01

0.02 <0.01 0.12 0.014

0.012 <0.012

0.041 0.021 0.022

0.012 <0.012 0.11 0.012

0.012 <0.012

0.012 0.012 0.012

0.012 <0.012 0.042 <0.012

<0.012 <0.012

<0.012 <0.012 <0.012

<0.012 <0.012 0.012 <0.008

<0.008 <0.008

<0.008 <0.008 <0.008

<0.008 <0.008 <0.008 0.063

<0.054 <0.054

0.11 <0.054 <0.054

<0.054 <0.054 0.28 Spain R 2004 0807/2 fruit

fruit, washed washings

APPLE SAUCE : strain rest

raw sauce

sauce APPLE JUICE : raw juice juice pomace, dried 21 0.10 0.06 0.02

0.27 0.06 0.04

0.03 0.01 0.41 0.015

0.077 0.020

0.34 0.070 0.043

0.042 0.012 0.50 0.041

0.032 0.012

0.057 0.038 0.032

0.027 0.024 0.20 0.028

0.021 <0.012

0.025 0.024 0.020

0.022 0.023 0.089 0.008

0.008 <0.008

0.008 0.008 <0.008

0.008 0.008 0.008 0.20

0.20 <0.054

0.70 0.20 0.13

0.13 0.078 1.2



### Based on the residue levels in the treated processi ng products transfer factors were calculated. The t ransfer factors for the processing products are calculated according to the following equation:

Transfer Factor = Residue concentration in the proc essed product [mg/kg] / Residue concentration in the RAC [mg/kg]

Transfer factors are calculated on a worst-case bas is. For this purpose, residues < LOQ are set at the LOQ. Average transfer factors of 0.6 and 0.8 could be ca lculated for the transfer of the total residue of B YI08330 from apple fruit into apple juice and apple sauce. The transfer factors are summarized in Table .8.1.2 -5. No transfer factors could be calculated for some proce ssed commodities from trial R 2004 0795/5, because the total residue of BYI08330 in fruit and in processed commodities was below the LOQ.

Table B.7.7.2.2.2-5: Transfer factors for the total residue of BYI08330 into processed commodities related to apple fruit

Transfer Factors for Total Residue of BYI08330

Sample material R 2004 0795/5 R 2004 0797/1 R 2004 0805/6 R 2004 08 07/2 mean

Fruit washed 1.2 0.6 0.9 1.0 0.9 Washing of apples washings Not calculated 0.6 0.9 0.3 0.6 Apple sauce processing Strain rest

(wet pomace) 2.4 2.1 1.7 3.6 2.5

### - 167 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Transfer Factors for Total Residue of BYI08330 Sample material R 2004 0795/5 R 2004 0797/1 R 2004 0805/6 R 2004 08 07/2 mean

Raw sauce (raw stewed fruit) 1.2 1.0 0.9 1.0 1.0

Sauce Not calculated 0.8 0.9 0.7 0.8 Raw juice Not calculated 0.6 0.9 0.7 0.7

Juice pasteurised Not calculated 0.6 0.9 0.4 0.6 Apple juice processing

Dried pomace 6.4 6.8 4.4 6.2 6.0



### Conclusion : As average transfer factors of 0.6 and 0.8 could be calculated for the transfer of the total residue o f BYI08330 from apple fruit into apple juice and appl e sauce, no concentration of BYI08330 is to be expe cted in these two commodities during processing. A mean factor of 2.5 was calculated for wet pomace, which is used for animal feed. Resulting from the individual data points of residue trials on apples the STMR ( 0.096 mg/lg) using the processing factor of 2.5 leads to a residue of 0.24 mg/kg in apple pomace, which cont ributes to the dietary burden.

B.7.7.2.2.3 Cherry Fruit Preserve

Reference: Determination of the residues of BYI 08330 in/on sw eet cherry fruit and the processed fractions (fruit washed, washings, fruit depitted, preserve) and sour cherry fruit and the processed fractions (frui t washed, washings, fruit de-pitted, preserve) after spraying of BYI 08330 (1 00 OD) in the field in Northern France and Germany Author(s), year: Schoening R., Helfrich P.; 2005 Report/Doc. number: RA-3119/04, including trials no . R 2004 0718/1, R 2004 0720/3, R 2004 0721/1, R 2004 0723/8 M-263882-01-1 Guideline(s): EU Council Directive 91/414/EEC of Ju ly15, 1991, Annex II, part A, section 6 and Annex III, part A, section 8: Residues in or on treated products, food and feed GLP: Yes. Deviations: None. Validity: The study is considered acceptable. The purpose of the presented study was to determine the transfer of BYI 08330 and its metabolites BYI08330-enol, BYI08330-ketohydroxy, BYI08330-mono- hydroxy and BYI08330-enol-Glc from sweet cherry and sour cherry (fruit, raw agricultural commodity) into sweet cherry and sour cherry processed fracti ons (fruit, washed; fruit, pitted; preserve) and by-pro ducts obtained during sweet and sour cherry process ing (washings).

Material and methods: Sweet and sour cherry samples from four field trial s that were performed in Germany and Northern Franc e in 2004 as part of study RA-2119/04 with BYI 08330 (10 0 OD) were processed. Information about the treated plots is given in Table B.7.7.2.2.3-1.

### - 168 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.7.2.2.3-1: Application Data Summary in/on Sweet and Sour Cherries in Northern Europe.

Country Trial No. Number Formulation Kg a.s./ha Kg a.s./ha x m *) Growth stage

BBCH

Northern France R 2004 0718/1 2 OD 100 0.144 0.072 73-75

Germany R 2004 0720/3 2 OD 100 0.180 0.072 76-78

Northern France R 2004 0721/1 2 OD 100 0.144 0.072 76-81

Germany R 2004 0723/8 2 OD 100 0.144 0.072 75

*) Rate per m height of leafy surface



### Preparation of processed fractions: The processing of washed fruit and pitted fruit sim ulated household practice (see Table B.7.7.2.2.3-2) . The processing of preserve simulated the industrial pra ctice at a laboratory scale.

Table B.7.7.2.2.3-2: Preparation of cherry (RAC) t o processed fractions: Processing of Fruit into Washed Fruit and Washing Water Processing of Cherry Fruit into Pitted Fruit and Preserve Stalks and damaged fruits were sorted out. The fruit s were washed for approx. 2 min in lukewarm standing water (ratio water/fruits = 2/1 (w/w)) by moving them aro und slowly. After washing, the fruits were let to drain in a sieve. Stalks and damaged fruits were sorted out. The fruit s were washed for 1 to 2 min in lukewarm standing water (r atio water/fruits = 2/1 (w/w)) by moving them around slo wly. After washing the fruits were let to drain in a siev e. The washed fruits were pitted by hand.

The pitted fruits remaining for further processing were filled into 1/1 preserving cans and sugar solution (w (sugar) = 0.14) was added. The preserving cans were pasteurised in an autoclave. After pasteurisation, the preserving cans were emptied in a larger vessel, mi xed thoroughly and weighed.



### Residues of BYI 08330 and its metabolites BYI08330- enol, BYI08330-ketohydroxy, BYI08330-mono-hydroxy and BYI08330-enol-Glc were determined by HPLC-ESIMS / MS according to method 00857 in/on sweet cherry and according to method 00857/E001 in/on sou r cherry (raw agricultural commodity, processed commodities and processing by-products). The Limit of Quantitation (LOQ), defined as the lowest validated fortification leve l (calculated as BYI 08330 equivalents), was 0.01 mg/kg (BYI 08330), 0.012 mg/ kg (BYI08330- enol, BYI08330-ketohydroxy, BYI08330- mono-hydroxy) and 0.008 mg/kg (BYI08330- enol-Glc) in/on sweet and sour cherry (raw agricultural commodity, processed commodities and processing by- products). The LOQ for the total residue of BYI 08330 (sum of single analyte residues, each calcula ted as BYI 08330 equivalents) was calculated as 0.0 54 mg/kg in/on sweet and sour cherry (raw agricultural commodity, processed commodities and processing by

products). Recovery results are summarized in Table B.7.7.2.2. 3-3.

Table B.7.7.2.2.3-3: Recovery results (concurrent recoveries) for determination of BYI 08330 and its metabolites in cherry fruit and in processed commod ities Sample Material Sweet Cherry Fruit Sweet Cherry Preserve Sour Cherry Fruit Sour Cherry Preserve

Analyte Forti-fication

levels *) Mean

Recovery [%±RDS] Forti-fication

levels Mean

Recovery [%±RDS] Fortification levels Mean

Recovery [%±RDS] Fortification levels Mean

Recovery [%±RDS] BYI 08330 0.01

1.0 92 ± 4.6

(n=12) 0.01

1.0 86

(n=2) 0.01

1.0 93 ± 5.6

(n=12) 0.01

1.0 93

(n=2)

### - 169 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Sample Material Sweet Cherry Fruit Sweet Cherry Preserve Sour Cherry Fruit Sour Cherry Preserve

Analyte Forti-fication

levels *) Mean

Recovery [%±RDS] Forti-fication

levels Mean

Recovery [%±RDS] Fortification levels Mean

Recovery [%±RDS] Fortification levels Mean

Recovery [%±RDS] BYI08330- enol 0.01

1.0 91 ± 12.5

(n=12) 0.01

1.0 86

(n=2) 0.01

1.0 92 ± 13.1

(n=12) 0.01

1.0 97

(n=2)

BYI08330-ketohydroxy 0.01

1.0 94 ± 6.9

(n=12) 0.01

1.0 88

(n=2) 0.01

1.0 95 ± 6.5

(n=12) 0.01

1.0 93

(n=2)

BYI08330-

monohydroxy 0.01

1.0 93 ± 5.3

(n=12) 0.01

1.0 88

(n=2) 0.01

1.0 94 ± 5.2

(n=12) 0.01

1.0 92

(n=2)

BYI08330- enol-Glc 0.01

1.0 93 ± 4.8

(n=12) 0.01

1.0 93

(n=2) 0.01

1.0 93 ± 4.6

(n=12) 0.01

1.0 92

(n=2)

*) levels refer to fortification with individual anal ytes (not calculated as BYI 08330 equivalents). 

### The mean of the recoveries were for all matrices an d for all fortification levels, within the acceptab le range of

70 – 110 %.

Findings: The total residue of BYI08330 in cherry fruit used for the processing studies was between 0.28 and 0.9 3 mg/kg. In washed fruit the total residue ranged fro m 0.25 to 0.83 mg/kg and in preserve from 0.13 to 0 .43 mg/kg. An average factor of 0.5 was calculated for the transfer of the total residue of BYI08330 from cherry fruit into cherry preserve. The residues results de termined in the different processed commodities are given in Table B.7.7.2.2.3-4.

Table B.7.7.2.2.3-4: Residues of BYI 08330 in cher ry fruit and in processed commodities Residues [mg/kg] Country / Trial No. Portion

analysed PHI

[days] BYI 08330 BYI 08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total Res.

of BYI 08330 calc.

Northern France R 2004 0718/1

Sweet Cherry fruit

fruit, washed washings fruit, pitted preserve 21 0.01 0.01 <0.01 0.01 0.01 0.32

0.30 <0.012 0.29 0.19 0.11

0.13 <0.012 0.077 0.044 0.12

0.12 <0.012 0.12 0.068 0.023

0.022 <0.008 0.020 0.012 0.57

0.59 <0.054 0.51 0.33

Germany R 2004 0720/3

Sour Cherry fruit

fruit, washed washings fruit, pitted preserve 21 0.01 0.01 <0.01 0.01 0.01 0.21

0.17 <0.012 0.20 0.087 0.033

0.036 <0.012 0.029 0.013 0.021

0.021 <0.012 0.029 0.012 0.011

0.011 <0.008 0.015 0.008 0.28

0.25 <0.054 0.28 0.13

Northern France R 2004 0721/1

Sweet Cherry fruit

fruit, washed washings fruit, pitted preserve 21 0.02 0.01 <0.01 0.01 0.01 0.58

0.51 <0.012 0.43 0.28 0.072

0.093 <0.012 0.050 0.032 0.17

0.14 <0.012 0.11 0.068 0.097

0.076 <0.008 0.058 0.034 0.93

0.83 <0.054 0.65 0.43

Germany R 2004 0723/8

Sour Cherry fruit

fruit, washed washings fruit, pitted preserve 21 <0.01 <0.01 <0.01 <0.01 <0.01 0.21

0.21 <0.012 0.18 0.10 0.012

0.019 <0.012 0.012 0.012 0.040

0.041 <0.012 0.037 0.019 0.023

0.023 <0.008 0.018 0.009 0.29

0.29 <0.054 0.25 0.14

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Based on the residue levels in the treated processi ng products transfer factors were calculated. The t ransfer factors for the processing products are calculated according to the following equation:

Transfer Factor = Residue concentration in the proc essed product [mg/kg] / Residue concentration in th e RAC [mg/kg]

Transfer factors are calculated on a worst-case bas is. For this purpose, residues < LOQ are set at the LOQ. Average transfer factors of 0.9 and 0.5 could be ca lculated for the transfer of the total residue of B YI08330 from cherry fruit into pitted fruit and preserve. T he transfer factors are summarized in Table B.7.7.2 .2.3-5.

Table B.7.7.2.2.3-5: Transfer factors for the tota l residue of BYI08330 into processed commodities related to cherry fruit

Transfer Factors for Total Residue of BYI08330 Sample material R 2004 0718/1 R 2004 0720/3 R 2004 0721/1 R 2004 07 23/8 mean

Fruit washed 1.0 0.9 0.9 1.0 1.0 Washing water 0.1 * 0.2 * 0.1 * 0.2 * 0.2 Fruit, pitted 0.9 1.0 0.7 0.8 0.9

Preserve 0.6 0.5 0.5 0.5 0.5

* Residues < LOQ are set to LOQ.



### Conclusion : As average transfer factors of 0.9 and 0.5 could be calculated for the transfer of the total residue o f BYI08330 from cherry fruit into pitted cherry fruit and cherry preserve, no concentration of BYI08330 is to be expected in these two commodities during processing

.

B.7.7.2.2.4 Raisins

Reference: Determination of the residues of BYI 08330 in the p rocessed fractions of grape, bunch of grapes for processing (raisin waste , washings, raisin) after spraying of BYI 08330 (150 OD) in the field in Spai n and Italy Author(s), year: Ballesteros C., Eberhard R.; 2006, amended 21.08.2006 Report/Doc. number: RA-3034/05, including trials no . R 2005 0157/9, R 2005 0158/7 M-271371-02-1 Guideline(s): EU Council Directive 91/414/EEC of Ju ly15, 1991, Annex II, part A, section 6 and Annex III, part A, section 8: Residues in or on tr eated products, food and feed GLP: Yes. Deviations: None. Validity: The mean of the concurrent recoveries wer e for all matrices and for all fortification levels, within the acceptable range of 70 – 110 %, except on grape raisin waste and grape raisin for BYI08330-enol-Glucoside, the r ecoveries were around 65 %, but with a low RSD these results were considered as valid. Consequently, all the results are regarded as valid. The purpose of the presented study was to determine the transfer of BYI 08330 and its metabolites BYI08330-enol, BYI08330-ketohydroxy, BYI08330-mono- hydroxy and BYI08330-enol-Glc from grape (bunch of grapes) into raisins and by-products obtained du ring processing (washing water and raisin waste).

Material and methods: The grape samples used for processing originated fr om two supervised field residue trials with grape i n Spain and Italy. A treated and an untreated plot we re used for each trial. Information about the treat ed plots

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

is given in Table B.7.7.2.2.4-1. The samples of bun ch of grape for processing were taken on day 7 afte r the last application.

Table B.7.7.2.2.4-1: Application Data Summary in/o n Grapes in Southern Europe.

Country Trial No. Number Formulation Kg a.s./ha Kg a.s./hL Growth stage

BBCH Spain R 2005 0157/9 2 OD 150 0.0960 0.01200 83 - 85

Italy R 2005 0158/7 2 OD 150 0.0960 0.00960 77 - 79



### Preparation of processed fractions: The processing of bunch of grapes into raisins simu lated the industrial practice at a laboratory scale

. Bunches of grapes were de-stemmed (separation into stalks and berries with stems) before drying in ord er to accelerate the drying process. The berries were dri ed at a temperature of 60 to 65°C in a fan-assisted oven in order to lower the water content to 6 to 13%. To calculate the weight of raisin waste (= stalks + stems) after drying, the stalks (A) were also drie d in the oven under the same conditions as the berries. Afte r drying, the stems (B) were removed from the berri es. The stems and the dried stalks were combined, yield ing the sample raisin waste (A + B). The dried berries were washed in lukewarm standing water, during the washing step, the dried berries absorbed water. The water content of the raisins af ter washing (typically between 13 and 24%) was 29.4 % (R 2005 0157/9 C), 21.4% (R 2005 0157/9 TA), 24.6% (R 2005 0157/9 TB), 20.3% (R 2005 0158/7 TA) and 20.6% (R 2005 0158/7 TB). The raisins and the washi ng water were sampled.

Residues of BYI08330 and its metabolites were deter mined by HPLC-ESI-MS/MS according to method 00857. The quantification was performed using a sta ble-labelled internal standard for each reference i tem. The Limit of Quantitation (LOQ), defined as the lowest validated fortification leve l (calculated as BYI 08330 equivalents), was 0.01 mg/kg (BYI 08330), 0.012 mg/ kg (BYI08330-enol, BYI08330-ketohydroxy, BYI08330- mono-hydroxy) and 0.008 mg/kg (BYI08330-enol-Glc) i n/on apple (fruit). The LOQ for the total residue o f BYI 08330 (sum of single analyte residues, each calcula ted as BYI 08330 equivalents) was calculated as 0.0 54 mg/kg in/on grapes (fruit and processed fractions). Storage period for samples: The processed samples were kept deep-frozen for 17 to 27 days prior to analysis (last extraction). The storage period of d eep-frozen samples of bunch of grapes was 112 and 1 26 days. Procedural recovery results are summarized in Table B.7.7.2.2.4-2.

Table B.7.7.2.2.4-2: Recovery results (concurrent recoveries) for determination of BYI 08330 and its metabolites in grapes and in processed commodities Sample Material Grape raisin waste Grape washings Gr ape raisin

Analyte Fortification levels *) Mean Recovery

[%±RDS] Fortification levels *) Mean Recovery

[%±RDS] Fortification levels *) Mean

Recovery [%±RDS]

BYI 08330 0.01

1.0 94 ± 11.5

(n=6) 0.01

1.0 98 ± 14.1

(n=6) 0.01

1.0 97 ± 12.4

(n=6)

BYI08330-enol 0.01

1.0 90 ± 2.2

(n=6) 0.01

1.0 95 ± 5.2

(n=6) 0.01

1.0 96 ± 1.5

(n=6)

BYI08330-ketohydroxy 0.01

1.0 90 ± 4.0

(n=6) 0.01

1.0 94 ± 8.1

(n=6) 0.01

1.0 93 ± 5.9

(n=6)

BYI08330-monohydroxy 0.01

1.0 89 ± 2.3

(n=6) 0.01

1.0 96 ± 6.8

(n=6) 0.01

1.0 92 ± 4.9

(n=6)

BYI08330-enolGlc 0.01

1.0 61 ± 7.4

(n=6) 0.01

1.0 95 ± 7.0

(n=6) 0.01

1.0 66 ± 5.2

(n=6)

*) levels refer to fortification with individual anal ytes (not calculated as BYI 08330 equivalents).

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The mean of the recoveries were for all matrices an d for all fortification levels, within the acceptab le range of 70 – 110 %; except on grape raisin waste and grape raisin for BYI08330-enol-Glucoside, the recoveries were around 65 %, but with a low RSD these results were considered as valid. Consequently, all the results are considered as valid.

Findings: The total residues of BYI08330 in bunch of grapes u sed for raisin productions were 0.16 and 0.45 mg/kg

, respectively. In raisins, the total residue of BYI0 8330 ranged between 0.23 and 1.6 mg/kg. Residue results are given in Table B.7.7.2.2.4-3.

Table B.7.7.2.2.4-3: Residues of BYI 08330 in grap es and in processed commodities Residues [mg/kg] Country / Trial No. Portion

analysed PHI

[days] BYI 08330 BYI 08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total Res.

of BYI 08330 calc. Spain R 2005 0157/9 Bunch of

grapes

Sample TA*: raisin waste washings raisin

Sample TB: raisin waste washings raisin 7 0.09

0.07 <0.01 <0.01

0.14 <0.01 0.02 0.03

0.24 <0.012 0.17

0.26 <0.012 0.17 0.02

0.087 <0.012 0.020

0.12 <0.012 0.021 <0.01

<0.012 <0.012 <0.012

<0.012 <0.012 <0.012 0.02

0.052 <0.008 0.032

0.063 <0.008 0.045 0.16

0.48 <0.054 0.23

0.63 <0.054 0.25 Italy R 2005 0158/7 Bunch of

grapes

Sample TA: raisin waste washings raisin

Sample TB: raisin waste washings raisin 7 0.11

0.44 0.02 0.25

0.54 0.02 0.21 0.22

0.57 0.029 0.86

0.39 0.016 0.69 0.028

0.21 <0.012 0.11

0.27 <0.012 0.085 0.014

<0.012 <0.012 <0.012

<0.012 <0.012 <0.012 0.082

0.18 0.032 0.34

0.17 0.016 0.33 0.45

1.5 0.089 1.6

1.5 0.062 1.4



### * TA and TB are two different samples from one trial.



### Based on the residue levels in the treated processi ng products transfer factors were calculated. The t ransfer factors for the processing products are calculated according to the following equation:

Transfer Factor = Residue concentration in the proc essed product [mg/kg] / Residue concentration in th e RAC [mg/kg]

Transfer factors are calculated on a worst-case bas is. For this purpose, residues < LOQ are set at the LOQ.

An average factor of 2.7 was calculated for the tra nsfer of total residue of BYI08330 from bunch of gr apes into raisins. The transfer factors for the total re sidue of BYI08330 in raisins and processed by-produ cts are summarised in Table B.7.7.2.2.4-4.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.7.2.2.4-4: Transfer factors for the tota l residue of BYI08330 into processed commodities related to bunch of grapes:

Transfer Factors for Total Residue of BYI08330 Sample material R 2005 0157/9 TA R 2005 0157/9

TB R 2005 0158/7

TA R 2005 0158/7

TB mean

Raisin waste 3.2 4.1 3.6 3.3 3.6 Washings 0.3 0.3 0.2 0.1 0.2

raisin 1.7 1.8 4.0 3.3 2.7



### Conclusion : Concentration is to be expected during processing o f grapes to raisins, as an average transfer factor of 2.7 could be calculated for the transfer of the total r esidue of BYI08330 from bunch of grapes into raisin

.

B.7.7.2.2.5 Wine

Reference: Determination of the residues of BYI 08330 in/on gr ape (bunch of grapes) and processed fractions (pomace grape, must, wine) after spraying of BYI 08330 (100 OD) in the field in Germany Author(s), year: Schöning R., Wolters, A; 2006 Report/Doc. number: RA-3048/04, including trials no . R 2004 0192/2, R 2004 0193/0 M-264725-01-1 Guideline(s): EU Council Directive 91/414/EEC of Ju ly15, 1991, Annex II, part A, section 6 and Annex III, part A, section 8: Residues in or on tr eated products, food and feed GLP: Yes. Deviations: None. Validity: The study is considered acceptable.

Reference: Determination of the residues of BYI 08330 in/on gr ape bunch of grapes and the processed fractions (pomace grape, must, wine) after spraying of BYI 08330 (100 OD) in the field in Italy Author(s), year: Schöning,R., Eberhard R.; 2006, am ended 06.03.2006 Report/Doc. number: RA-3049/04, including trials no . R 2004 0196/5, R 2004 0197/3 M-263874-02-1 Guideline(s): EU Council Directive 91/414/EEC of Ju ly15, 1991, Annex II, part A, section 6 and Annex III, part A, section 8: Residues in or on tr eated products, food and feed GLP: Yes. Deviations: None. Validity: The study is considered acceptable.

The purpose of the presented studies was to determi ne the transfer of BYI 08330 and its metabolites (BYI08330-enol, BYI08330-ketohydroxy, BYI08330-mono -hydroxy and BYI08330-enol-Glc) from grape (bunch of grapes) into processed commodities (pomac e, grape; must; wine).

Material and methods: Grape samples from two field trials performed in Ge rmany as part of study RA-2048/04 with BYI 08330 (1 00 OD) and from two field trials performed in Italy as part of study RA-2049/04 with BYI 08330 (100 OD) w ere processed. Representative samples of the raw agricu ltural commodity and processed commodities were analysed for residues of BYI 08330 and its metaboli tes.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

The samples of bunch of grape for processing were t aken on day 7 after the last application. A treated and an untreated plot were used for each trial. Informa tion about the treated plots is given in Tables B.7 .8.1.5-1 and B.7.7.2.2.5-2, respectively.

Table B.7.7.2.2.5-1: Application Data Summary in/o n Grapes in Northern Europe.

Country Trial No. Number Formulation Kg a.s./ha Kg a.s./hL Growth stage

BBCH Germany R 2004 0192/2

red grape variety: Portugieser 2 OD 100 0.0720 0.00900 83 - 89

Germany R 2004 0193/0

white grape variety: Mueller Thurgau 2 OD 100 0.0720 0.00900 85



### Preparation of processed fractions from the Norther n European trials: The fresh bunch of grapes samples were weighed and subsequently crushed in a grape crusher. The mash obtained was pressed in a cloth press, while the pr essure was increased step by step from 0.2 to 2.0 b ar. After pressing, the pomace was sampled and stored d eep-frozen. The must was filled into vessels and 0. 1 g/L of potassium hyposulfite was added. To prevent a later protein haze in the wine, 1 g/L of the fini ng agent bentonite was added to the wine. After clarifying t he must was decanted from the lees. A sample of the must was taken and stored deep-froz en. The fermentation was started by the addition of 20 g / 100 L pure-culture yeast to the must. During th e fermentation the loss of weight due to the conver sion of sugar into CO2 was monitored in trial R 2004 0192/2 . After fermentation (approximately 1 month later), the first racking was effected. The yeast sediment was removed and after sulphating (125 mg/L) of the youn g wine the finishing of the wine was started. Approxi mately 3 months later the wine was filtered and dee pfrozen. Storage period for samples : The storage period of deep-frozen samples ranged between 56 and 170 days.

Table B.7.7.2.2.5-2: Application Data Summary in/o n Grapes in Southern Europe.

Country Trial No. Number Formulation Kg a.s./ha Kg a.s./hL Growth stage

BBCH Italy R 2004 0196/5

white grape variety: Chardonnay 2 OD 100 0.0960 0.00640 81 - 75

Italy R 2004 0197/3

red grape variety: Lambrusco di Sorbara 2 OD 100 0.0960 0.00640 83

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Preparation of processed fractions from the Souther n European trials: Preparation of grape pomace, must and white wine: Pre paration of grape pomace, must and red wine: The deep-frozen sample of bunch of grapes originati ng from trial R 2004 0196/5 was allowed to thaw at 2.5 °C. The partly thawn grape sample was weighed and subsequently crushed in a grape crusher. The mash obtained was pressed in a cloth press, while the pressure was increased step by step from 0.2 to 2.0 bar. Afte r pressing, part of the pomace was sampled and stored deep-frozen. The must was filled into vessels and 0.1 g/L of potassium hyposulfite was added. To prevent a later protein h aze in the wine, 1 g/L of the fining agent bentonite was a dded to the must. After clarifying, the must was decanted fr om the lees. A sample of the must was taken and stored deep

frozen. The fermentation was started by the addition of of pureculture yeast to the must. During fermentation , the loss of weight due to the conversion of sugar into CO 2 was monitored. After fermentation, the first racking was performed. The yeast sediment was removed and after sulphiting of the young wine the finishing of the w ine was started. Approximately 2 months later, 2 nd racking was done; the wine was filtered and deep-frozen. The grapes originating from trial R 2004 0197/3 wer e allowed to thaw at 2.5 °C. The partly thawn grape s ample was weighed and subsequently crushed and de-stemmed in a grape crusher. A mash heating was performed by heating up the obtained mash with steam to a temperature of T = 78 °C for 3 min while stirring. The mash was allowed to cool down. The mash was pressed in a cloth press, while increasing the pressure step by step from 0.2 to 2.0 bar. The labo ratory sample of grape pomace was prepared by filling a po rtion of the grape pomace in polystyrene boxes. The must was filled into vessels and a hyposulfite solution was added. To prevent a later protein haze in the w ine, 1 g/L of the fining agent bentonite was added to the wine. The must was allowed to clarify. After clarifying ov ernight, the must was decanted from the lees. The laboratory sample of must was prepared by filling a portion of the freshly decanted must in polystyrene boxes. The den sity of the obtained must was determined. The density of th e must amounted to an Oechsle value of 67; therefore no sugar was added prior to fermentation. The fermentation was started by addition of pure-cu lture yeast to the must. During fermentation, the loss of weight due to the conversion of sugar into CO 2 was monitored. The first racking was done 19 days after start of fermentation. After removal of the yeast sediment, potassium hyposulfite was added to the young wine a nd the finishing of the wine was started. Second racki ng was done about 2 months later. The wine was filtered an d the laboratory sample of wine was prepared by filling a portion of the wine in polystyrene boxes directly after fil tration. The laboratory samples were stored deep-frozen at -18 ° C or below. Comment RMS : The reported procedure is not representative for vinification of red wine, as the fermentation of red grapes takes place while the mu st is still on the mash (“Fermentation on skins”)



### Storage period for samples : The processed samples were kept deep-frozen for 1 9 or 20 days (wine) and 96 to 98 days (pomace, grape; must) prior to analysis (last extraction). The storage period of deep-froze n samples of bunch of grapes was 192 or 222 days.

Residues of BYI08330 and its metabolites were deter mined by HPLC-ESI-MS/MS according to method 00857. The quantification was performed using a sta ble-labelled internal standard for each reference i tem. The Limit of Quantitation (LOQ) , defined as the lowest validated fortification lev el (calculated as BYI 08330 equivalents), was 0.01 mg/kg (BYI 08330), 0.012 mg/ kg (BYI08330-enol, BYI08330-ketohydroxy, BYI08330- mono-hydroxy) and 0.008 mg/kg (BYI08330-enol-Glc) i n/on apple (fruit). The LOQ for the total residue o f BYI 08330 (sum of single analyte residues, each cal culated as BYI 08330 equivalents) was calculated as 0.054 mg/kg in/on grapes (fruit and processed fract ions). Procedural recovery results are summarized in Table B.7.7.2.2.5-3.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.7.2.2.5-3: Recovery results (concurrent recoveries) for determination of BYI 08330 and its metabolites in grapes and in processed commodities Sample Material Bunch of grapes Grape pomace Must Wine

Analyte Fortification levels *) Mean

Recovery [%±RDS] Fortification levels Mean

Recovery [%±RDS] Fortification levels Mean

Recovery [%±RDS] Fortification levels Mean

Recovery [%±RDS] BYI 08330 0.01

1.0 90 ± 9.6

(n=29) 0.01

1.0 92 ± 5.2

(n=8) 0.01

1.0 94 ± 6.2

(n=10) 0.01

1.0 94 ± 5.1

(n=8)

BYI08330- enol 0.01

1.0 93 ± 10.0

(n=29) 0.01

1.0 95 ± 5.0

(n=8) 0.01

1.0 96 ± 6.6

(n=10) 0.01

1.0 97 ± 2.1

(n=8)

BYI08330-ketohydroxy 0.01

1.0 94 ± 9.8

(n=29) 0.01

1.0 94 ± 5.3

(n=8) 0.01

1.0 95 ± 7.3

(n=10) 0.01

1.0 93 ± 5.5

(n=8)

BYI08330-

monohydroxy 0.01

1.0 92 ± 9.0

(n=29) 0.01

1.0 91 ± 2.7

(n=8) 0.01

1.0 92 ± 4.4

(n=10) 0.01

1.0 94 ± 4.1

(n=8)

BYI08330- enol-Glc 0.01

1.0 94 ± 8.4

(n=29) 0.01

1.0 88 ± 8.0

(n=8) 0.01

1.0 92 ± 4.5

(n=10) 0.01

1.0 92 ± 2.0

(n=8)

*) levels refer to fortification with individual anal ytes (not calculated as BYI 08330 equivalents). 

### The mean of the recoveries were for all matrices an d for all fortification levels, within the acceptab le range of 70 – 110 %;

Findings: In bunch of grapes used for wine production the tot al residue of BYI08330 was between 0.21 and 0.54 mg/kg. The total residue of BYI 08330 in wine was 0 .12 – 0.24 mg/kg. Residue results are given in Tabl e B.7.7.2.2.5-4.

Table B.7.7.2.2.5-4: Residues of BYI 08330 in grap es and in processed commodities Residues [mg/kg] Country / Trial No. Portion

analysed PHI

[days] BYI 08330 BYI 08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total Res.

of BYI 08330 calc. Germany R 2004 0192/2 Bunch of grapes

Pomace Must Wine 7 0.15 0.25 0.10 0.01 0.073

0.17 0.064 0.13 0.012

0.012 0.012 0.012 <0.012

0.012 <0.012 <0.012 0.024

0.039 0.023 0.018 0.25

0.48 0.20 0.17 Germany R 2004 0193/0 Bunch of grapes

Pomace Must Wine 7 0.15 0.21 0.05 0.06 0.036

0.092 0.021 0.11 0.012

0.021 0.012 0.012 <0.012

<0.012 <0.012 <0.012 0.011

0.028 0.008 0.008 0.21

0.36 0.091 0.19 Italy R 2004 0196/5 Bunch of grapes

Pomace Must Wine 7 0.15 0.25 0.10 0.03 0.17

0.32 0.054 0.090 0.095

0.24 0.077 0.065 0.012

0.020 <0.012 <0.012 0.11

0.12 0.056 0.048 0.54

0.95 0.29 0.24 Italy R 2004 0197/3 Bunch of grapes

Pomace Must Wine 7 0.20 0.44 0.11 0.04 0.045

0.077 0.034 0.048 0.045

0.056 0.031 0.017 <0.012

<0.012 <0.012 <0.012 0.026

0.024 0.020 0.013 0.32

0.60 0.20 0.12



### Based on the residue levels in the treated processi ng products transfer factors were calculated. The t ransfer factors for the processing products are calculated according to the following equation:

Transfer Factor = Residue concentration in the proc essed product [mg/kg] / Residue concentration in th e RAC [mg/kg]

Transfer factors are calculated on a worst-case bas is. For this purpose, residues < LOQ are set at the LOQ.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

An average transfer factor of 0.6 could be calculat ed for the transfer of the total residue of BYI0833 0 from bunch of grapes into must and wine. The transfer fa ctors for the total residue of BYI 08330 in wine an d the processed by-products are summarised in Table B.7.7 .2.2.5-5.

Table B.7.7.2.2.5-5: Transfer factors for the tota l residue of BYI08330 into processed commodities related to bunch of grapes:

Transfer Factors for Total Residue of BYI08330 Sample material R 2004 0192/2 R 2004 0193/0 R 2004 0196/5 R 2004 01 97/3 mean Pomace, grape 0.9 1.7 1.8 1.9 1.8

Must 0.8 0.4 0.5 0.6 0.6

Wine 0.7 0.9 0.4 0.4 0.6



### Conclusion : As an average transfer factor of 0.6 could be calcu lated for the transfer of the total residue of BYI0 8330 from bunch of grapes into must and wine, no concentratio n of BYI08330 is to be expected in these two commodities during processing.

B.7.7.2.2.6 Tomato juice, preserve and puree

Reference: Determination of the residues of BYI 08330 in/on to mato fruit and the processed fractions (washings, fruit peeled, raw ju ice, juice, strain rest, preserve, puree, fruit washed, raw puree, peel wash ed, peeling water) after spraying of BYI 08330 (100 OD) in the greenhouse in Greece, Spain and Italy Author(s), year: Freitag, T., Helfrich, P.; 2006 Report/Doc. number: RA-3140/04, including trials no . R 2004 0827/7, R 2004 0828/5, R 2004 0829/3, R 2004 0830/7 M-263490-01-1 Guideline(s): EU Council Directive 91/414/EEC of Ju ly15, 1991, Annex II, part A, section 6 and Annex III, part A, section 8: Residues in or on tr eated products, food and feed GLP: Yes. Deviations: None. Validity: The study is considered acceptable. The purpose of the presented study was to determine the transfer of BYI 08330 and its metabolites (BYI08330-enol, BYI08330-ketohydroxy, BYI08330-mono -hydroxy and BYI08330-enol-Glc) from tomato fruits into processed fractions after processing of tomato fruits to juice, preserve and puree.

Material and methods: Tomato samples from four supervised greenhouse resi due trials performed in Greece, Spain and Italy wit h BYI 08330 (100 OD) were processed. A treated and an untreated plot were used for each trial. Representative samples of the raw agricultural comm odity and processed commodities were analysed for residues of BYI 08330 and its metabolites. Informat ion about the treated plots is given in Table B.7.7 .2.2.6-1.

Table B.7.7.2.2.6-1: Application Data Summary in/o n Tomato in Greenhouse:

Country Trial No. Number Formulation Kg a.s./ha Kg a.s./ha x m *) Growth stage

BBCH

Greece R 2004 0827/7 4 OD 100 0.1080 - 0.1188 0.072 73-81

Spain R 2004 0828/5 4 OD 100 0.1152 0.072 81-85

Spain R 2004 0829/3 4 OD 100 0.1340 – 0.1440 0.072 84-87

### - 178 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Country Trial No. Number Formulation Kg a.s./ha Kg a.s./ha x m *) Growth stage

BBCH Italy R 2004 0830/7 4 OD 100 0.1044 – 0.1440 0.072 71 - 72

*) Rate per m height of leafy surface



### Preparation of processed fractions: The processing procedures simulated the industrial practice at a laboratory scale (see Table B.7.7.2.2 .6-2). For the preparation of examination samples, the dee p-frozen field sub-samples were shredded with dry i ce in

a cutter.

Table B.7.7.2.2.6-2: Preparation of tomato (RAC) t o processed fractions: Preparation of Washed Fruits, Washing water (Washings), Raw Juice and Juice Preparation of Peeled Tomatoes, Peeling Water, Peel and Preserves Preparation of Raw Puree, Puree and Wet Pomace

The tomatoes were washed in lukewarm standing water. Then samples of the washing water (washings ) and the washed tomato fruits were taken. The remaining washed tomatoes were cut with a knife into small pieces. The cut tomatoes were heated to prevent enzymatic reactions. After this blanching process, the tomato pulp was passed through a strainer to separate raw juice and wet pomace. Sodium chloride was added to the raw juice. Then samples of the raw juice were taken. One part of the remaining raw juice was used for the processing into preserves. The rest of the remaining raw juice was pasteurised . After pasteurisation the juice was sampled. Portions of the washing water (washings), washed fruits, raw juice and juice were stored deep-frozen at - 18°C or below until preparation of the examination samples. The deep-frozen tomatoes were washed in luke-warm standing water. After a few minutes the peel could be taken off. Samples of peel , peeling water and peeled fruits were taken. To another part of the remaining peeled tomatoes, raw juice was added. Then the tomato preserves were pasteurised . After pasteurisation, the tomato preserves were sampled. Portions of the peeling water, peel, peeled fruits and of the preserves were stored deep-frozen at -18°C or below until preparation of the examination samples The tomatoes were washed in lukewarm standing water. The washed tomatoes were cut with a knife into small pieces. The cut tomatoes were heated to prevent enzymatic. After this blanching process, the tomato pulp was passed through a strainer to separate raw juice and wet pomace. The wet pomace was sampled. After addition of sodium chloride, the raw juice was separated into raw puree and tomato liquid by centrifugation. The tomato raw puree was sampled. A part of the remaining raw puree was filled into 1/1 preserving cans and pasteurised

. After pasteurisation the puree was sampled. Portions of pomace wet, raw puree and puree were stored deep-frozen at -18°C or below until preparation of the examination samples.



### Storage period for samples : The storage period of deep-frozen samples ranged between 14 and 298 days.

Residues of BYI 08330 and its metabolites BYI08330- enol, BYI08330-ketohydroxy, BYI08330-mono-hydroxy and BYI08330-enol-Glc in/on tomato (fruit) and proc essed fractions were determined by HPLC-ESI-MS/MS according to method 00857. The Limit of Quantitation (LOQ) , defined as the lowest validated fortification lev el (calculated as BYI 08330 equivalents), was 0.01 mg/kg (BYI 08330), 0.012 mg/ kg (BYI08330-enol, BYI08330-ketohydroxy, BYI08330- mono-hydroxy) and 0.008 mg/kg (BYI08330-enol-Glc) i n/on tomato (fruit) and processed fractions. The LO Q for the total residue of BYI 08330 (sum of single a nalyte residues, each calculated as BYI 08330 equiv alents) was calculated as 0.054 mg/kg in/on tomato (fruit) and processed fractions Procedural recovery results are summarized in Table B.7.7.2.2.6-3.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.7.2.2.6-3: Recovery results (concurrent recoveries) for determination of BYI 08330 and its metabolites in tomato and in processed commodities Sample Material Fruit 1) Preserve 2) Juice 3)

Analyte Forti-fication levels *) Mean Recovery

[%±RDS] Forti-fication levels *) Mean Recovery

[%±RDS] Forti-fication levels *) Mean Recovery

[%±RDS] BYI 08330 0.01

1.0 2.0 90 ± 7.8

(n=30) 0.01

1.0 89 ± 8.8

(n=12) 0.01

1.0 92 ± 9.8

(n=12)

BYI08330-enol 0.01

1.0 2.0 93 ± 12.5

(n=30) 0.01

1.0 87 ± 10.6

(n=12) 0.01

1.0 91 ± 11.3

(n=12)

BYI08330-ketohydroxy 0.01

1.0 2.0 93 ± 6.6

(n=30) 0.01

1.0 94 ± 7.2

(n=12) 0.01

1.0 99 ± 6.3

(n=12)

BYI08330-monohydroxy 0.01

1.0 2.0 93 ± 7.1

(n=30) 0.01

1.0 93 ± 7.7

(n=12) 0.01

1.0 97 ± 9.2

(n=12)

BYI08330-enolGlc 0.01

1.0 2.0 97 ± 7.4

(n=30) 0.01

1.0 94 ± 8.6

(n=12) 0.01

1.0 100 ± 10.3

(n=12)

*) levels refer to fortification with individual anal ytes (not calculated as BYI 08330 equivalents). 1) sample material fruit covers sample materials fr uit washed, fruit peeled, peel washed. 2) sample material preserve covers sample materials strain rest (pomace wet), raw puree and puree 3) sample material juice covers sample materials ra w juice, washings (washing water) and peeling water



### The mean of the recoveries were for all matrices an d for all fortification levels, within the acceptab le range of 70 – 110 %;

Findings: The total residue of BYI08330 in tomato fruit was b etween 0.2 and 0.5 mg/kg. The total residue in juic e ranged between 0.13 and 0.3 mg/kg, in preserve betw een 0.1 and 0.35 mg/kg, and in puree between 0.13 and 0.59 mg/kg. The residue results are summarised in Table B.7.7.2 .2.6-4.

Table B.7.7.2.2.6-4: Residues of BYI 08330 in toma toes and in processed commodities Residues [mg/kg] Country / Trial No. Portion

analysed PHI

[days] BYI 08330 BYI 08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total Res.

of BYI 08330 calc.

Greece R 2004 0827/7 Fruit

washings fruit, peeled raw juice juice

strain rest preserve puree

fruit, washed raw puree

peel, washed peeling water 3 0.06 <0.01 <0.01 <0.01 <0.01

<0.01 <0.01 <0.01

0.01 <0.01

0.04 0.01 0.39

<0.012 0.30 0.29 0.27

0.62 0.31 0.55

0.29 0.57

0.30 0.066 0.021

<0.012 0.012 0.012 0.012

0.027 0.012 0.022

0.014 0.022

0.032 0.012 <0.012

<0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012

<0.012 <0.012

<0.012 <0.012 0.031

<0.008 0.030 0.022 0.018

0.025 0.028 0.019

0.018 0.022

0.008 0.008 0.50

<0.054 0.34 0.32 0.30

0.67 0.35 0.59

0.33 0.61

0.38 0.096

### - 180 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues [mg/kg] Country / Trial No. Portion

analysed PHI

[days] BYI 08330 BYI 08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total Res.

of BYI 08330 calc. Spain R 2004 0828/5 Fruit

washings fruit, peeled raw juice juice

strain rest preserve puree

fruit, washed raw puree

peel, washed peeling water 3 0.09 <0.01 <0.01 0.02 0.01

0.10 0.01 0.01

0.05 0.04

0.78 0.02 0.10

<0.012 0.058 0.098 0.10

0.23 0.072 0.18

0.090 0.15

0.17 0.012 0.012

<0.012 <0.012 0.012 0.012

0.012 <0.012 0.012

0.012 0.012

0.034 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012

<0.012 <0.012

<0.012 <0.012 0.043

<0.008 0.028 0.028 0.022

0.027 0.021 0.026

0.030 0.030

0.021 0.008 0.25

<0.054 0.086 0.16 0.14

0.36 0.10 0.23

0.19 0.23

1.0 <0.054 Spain R 2004 0829/3 Fruit

washings fruit, peeled raw juice juice

strain rest preserve puree

fruit, washed raw puree

peel, washed peeling water 3 0.15 0.02 <0.01 0.01 <0.01

0.02 <0.01 <0.01

0.04 0.01

0.18 0.04 0.11

0.021 0.050 0.12 0.11

0.23 0.075 0.13

0.091 0.12

0.044 0.012 0.012

<0.012 <0.012 0.012 0.012

0.012 <0.012 0.012

0.012 0.012

0.012 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012

<0.012 <0.012

<0.012 <0.012 0.052

<0.008 0.029 0.033 0.025

0.029 0.028 0.023

0.064 0.026

0.010 0.008 0.32

<0.054 0.079 0.17 0.15

0.29 0.10 0.17

0.21 0.17

0.24 0.061 Italy R 2004 0830/7 Fruit

washings fruit, peeled raw juice juice

strain rest preserve puree

fruit, washed raw puree

peel, washed peeling water 3 0.07 <0.01 0.01 0.01 <0.01

0.02 <0.01 <0.01

0.02 0.01

0.22 0.01 0.093

<0.012 0.057 0.096 0.10

0.20 0.092 0.10

0.063 0.14

0.084 0.012 0.012

<0.012 <0.012 0.012 0.012

0.012 0.012 0.012

0.012 0.012

0.031 <0.012 <0.012

<0.012 <0.012 <0.012 <0.012

<0.012 <0.012 <0.012

<0.012 <0.012

<0.012 <0.012 0.028

<0.008 0.023 0.022 0.018

0.018 0.021 0.012

0.018 0.019

0.008 <0.008 0.20

<0.054 0.090 0.14 0.13

0.25 0.13 0.13

0.11 0.18

0.34 <0.054



### Based on the residue levels in the treated processi ng products transfer factors were calculated. The t ransfer factors for the processing products are calculated according to the following equation:

Transfer Factor = Residue concentration in the proc essed product [mg/kg] / Residue concentration in th e RAC [mg/kg]

Transfer factors are calculated on a worst-case bas is. For this purpose, residues < LOQ are set at the LOQ.

Average transfer factors of 0.6, 0.5 and 0.9 could be calculated for the transfer of the total residue of BYI08330 from tomato fruit into juice, preserve and puree, respectively

. The transfer factors for the total residue of BYI 08330 in tomato and the processed by -products are summarised in Table B.7.7.2.2.6-5.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.7.2.2.6-5: Transfer factors for the tota l residue of BYI08330 into processed commodities related to tomato fruit:

Transfer Factors for Total Residue of BYI08330 Sample material R 2004 0827/7 R 2004 0828/5 R 2004 0829/3 R 2004 08 30/7 mean

Juice Production :

fruit washed washings raw juice juice 0.7 0.1 *)

0.6 0.6 0.8

0.2 *)

0.6 0.6 0.7

0.2 *)

0.5 0.5 0.6

0.3 *)

0.7 0.7 0.7

0.2 0.6 0.6 Preserve Production :

fruit peeled peel washed peeling water preseve 0.7 0.8 0.2 0.7 0.3

4.0 0.2 *)

0.4 0.2

0.8 0.2 0.3 0.5

1.7 0.3 *)

0.7 0.4

1.8 0.2 0.5

Puree Production

strain rest (wet pomace) puree raw puree 1.3 1.2 1.2 1.4

0.9 0.9 0.9

0.5 0.5 1.3

0.7 0.9 1.2

0.8 0.9

*) For calculation of the transfer factor the resid ue in the processed fraction was set at LOQ.



### Conclusion: As the average transfer factors resulting from toma to processing into juice, preserve and puree were < 1.0, no concentration of BYI08330 is to be expected in t hese commodities during processing.

B.7.7.2.2.7 Cooked beans

Reference: Determination of the residues of BYI 08330 in/on cl imbing French bean (beans with pod) and the processed fractions (washi ngs, cooking water, bean cooked, bean washed) after spraying of BYI 083 30 (100 OD) in the greenhouse in Italy, Germany and southern France Author(s), year: Schöning R., Billian P., Wolters, A.; 2006 Report/Doc. number: RA-3042/04, including trials no . R 2004 0172/8, R 2004 0173/6, R 2004 0174/4, R 2004 0175/2 M-263683-01-1 Guideline(s): EU Council Directive 91/414/EEC of Ju ly15, 1991, Annex II, part A, section 6 and Annex III, part A, section 8: Residues in or on tr eated products, food and feed GLP: Yes. Deviations: None. Validity: The study is considered acceptable. The purpose of the presented study was to determine the transfer of BYI 08330 and its metabolites (BYI08330-enol, BYI08330-ketohydroxy, BYI08330-mono -hydroxy and BYI08330-enol-Glc) from Climbing French bean (bean with pod, raw agricultural commod ity) into Climbing French bean processed commoditie s (bean, cooked; bean with pod, washed) and by-produc ts obtained during Climbing French bean processing (washings; cooking water).

Material and Method: Climbing French Bean samples from four greenhouse t rials that were performed in Italy, Germany and Southern France as part of study RA-2042/04 with BY I 08330 (100 OD) were processed. Representative samples of the raw agricultural commodity, processe d commodities and processing by-products were analysed for residues of BYI 08330 and its metaboli tes. Information about the treated plots is given in Tab le B.7.7.2.2.7-1.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.7.2.2.7-1: Application Data Summary in/o n French beans in Greenhouse:

Country Trial No. Number Formulation Kg a.s./ha Kg a.s./ha x m *) Growth stage

BBCH Italy R 2004 0172/8 4 OD 100 0.0864 - 0.1440 0.072 51-71

Italy R 2004 0173/6 4 OD 100 0.1440 0.072 71-76

Germany R 2004 0174/4 4 OD 100 0.1440 0.072 69-78

Southern France R 2004 0175/2 4 OD 100 0.1260 0.072 65-79

*) Rate per m height of leafy surface



### Climbing French bean samples (bean with pod) were t aken from the treated and the control plots on day 14 after the last application.The field samples from a ll trials were stored deep-frozen within 24 hours a fter sampling. Preparation of processed fractions: Processing of the Climbing French bean samples into washed beans with pod, washing water, cooked beans with pod and cooking water was performed. The washi ng and cooking of Climbing French beans was done using household practice (see Table B.7.7.2.2.7-2).

Table B.7.7.2.2.7-2: Preparation of Climbing Frenc h bean with pod (RAC) to processed fractions: Preparation of Washed Climbing Beans and Washing Water Preparation of Cooked Climbing Beans and Cooking Water The beans were washed in lukewarm standing water. After washing, the beans were let to drain in a siev e. A portion of the washed beans and of the washing water was stored deep-frozen at -18°C or below until preparat ion of the examination samples. Both ends of the remaining washed beans were removed

, and the beans were cut in small pieces (approx. 3 – 6 cm). Subsequently, the washed and cut beans were cooked f or about 15 – 20 min in salt water. After cooking, the beans were let to drain in a siev e. A portion of the cooked beans and of the cooking water was stored deep-frozen at-18°C or below until preparati on of the examination samples.



### Residues of BYI 08330 and its metabolites BYI08330- enol, BYI08330-ketohydroxy, BYI08330-mono-hydroxy and BYI08330-enol-Glc in/on Climbing French bean (r aw agricultural commodity, processed commodities and processing by-products) were determined by HPLC -ESI-MS/MS according to method 00857/E001. The Limit of Quantitation (LOQ) , defined as the lowest validated fortification lev el (calculated as BYI 08330 equivalents), was 0.01 mg/kg (BYI 08330), 0.012 mg/ kg (BYI08330-enol, BYI08330-ketohydroxy, BYI08330- mono-hydroxy) and 0.008 mg/kg (BYI08330-enol-Glc) i n/on Climbing French bean (raw agricultural commodity, processed commodities and processing by- products). The LOQ for the total residue of BYI 08330 (sum of single analyte residues, each calcula ted as BYI 08330 equivalents) was calculated as 0.054 mg/kg in/on Climbing French bean. Procedural recovery results are summarized in Table B.7.7.2.2.7-3.

Table B.7.7.2.2.7-3: Recovery results (concurrent recoveries) for determination of BYI 08330 and its metabolites in Climbing French bean and in processe d commodities Sample material Bean with pod Washings Analyte Fortification levels *) Mean Recovery [%±RSD] Fortification levels *) Mean Recovery [%±RSD] BYI 08330 0.01 2.0 92 ± 5.4

(n=19) 0.01 1.0 92 ± 5.4 (n=6)

BYI08330-enol 0.01 2.0 88 ± 6.6

(n=19) 0.01 1.0 86 ± 12.5 (n=6)

### - 183 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Sample material Bean with pod Washings Analyte Fortification levels *) Mean Recovery [%±RSD] Fortification levels *) Mean Recovery [%±RSD] BYI08330-keto-hydroxy 0.01 2.0 94 ± 4.7

(n=19) 0.01 1.0 94 ± 7.5 (n=6) BYI08330-mono-hydroxy 0.01 2.0 94 ± 4.9

(n=19) 0.01 1.0 95 ± 6.0 (n=6) BYI08330-enol-Glc 0.01 2.0 96 ± 9.8

(n=19) 0.01 1.0 99 ± 11.1 (n=6)

*) levels refer to fortification with individual anal ytes (not calculated as BYI 08330 equivalents).



### Recoveries for bean (cooked) and bean with pod (was hed) were covered by the recoveries determined for bean with pod. Recoveries for cooking water were co vered by the recoveries determined for washings. Th e mean of the recoveries were for all matrices and fo r all fortification levels, within the acceptable r ange of 70 – 110 %;

Findings: The total residue of BYI08330 in beans with pod was between 0.11 and 0.57 mg/kg. The total residue in washed beans ranged between 0.076 and 0.47 mg/kg an d in cooked beans between 0.07 and 0.31 mg/kg. The results are summarised in Table B.7.7.2.2.7-4.

Table B.7.7.2.2.7-4: Residues of BYI 08330 in Clim bing French bean and in processed commodities Residues [mg/kg] Country / Trial No. Portion

analysed PHI

[days] BYI 08330 BYI 08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total Res.

of BYI 08330 calc. Italy R 2004 0172/8 Bean with pod

washings cooking water bean cooked bean with pod washed 14 0.06 <0.01 <0.01 <0.01 0.04 0.12

0.023 0.061 0.076 0.12 0.081

<0.012 0.012 0.012 0.046 0.012

<0.012 <0.012 <0.012 0.012 0.030

<0.008 0.008 0.010 0.022 0.31

<0.054 0.081 0.097 0.23

Italy R 2004 0173/6 Bean with pod

washings cooking water bean cooked bean with pod washed 14 0.01 <0.01 <0.01 <0.01 0.01 0.066

<0.012 0.029 0.052 0.019 0.020

<0.012 0.012 0.012 0.038 <0.012

<0.012 <0.012 <0.012 <0.012 0.008

<0.008 0.008 0.008 0.008 0.11

<0.054 <0.054 0.071 0.076

Germany R 2004 0174/4 Bean with pod

washings cooking water bean cooked bean with pod washed 14 0.13 * 0.01 <0.01 <0.01 0.06 0.29 *

0.044 0.12 0.24 0.24 0.099 *

0.012 0.014 0.025 0.079 0.012 *

<0.012 <0.012 <0.012 0.012 0.035 *

<0.008 0.009 0.015 0.027 0.57 *

0.066 0.14 0.28 0.42

Southern France R 2004 0175/2 Bean with pod

washings cooking water bean cooked bean with pod washed 14 0.15 * 0.01 <0.01 <0.01 0.10 0.26 *

0.036 0.15 0.25 0.23 0.099 *

0.012 0.018 0.029 0.089 0.012 *

<0.012 0.012 0.012 0.012 0.043 *

<0.008 0.012 0.020 0.037 0.57 *

0.058 0.19 0.31 0.47

* Measurement in duplicate



### Based on the residue levels in the treated processi ng products transfer factors were calculated. The t ransfer factors for the processing products are calculated according to the following equation:

Transfer Factor = Residue concentration in the proc essed product [mg/kg] / Residue concentration in th e RAC [mg/kg]

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Transfer factors are calculated on a worst-case bas is. For this purpose, residues < LOQ are set at the LOQ.

Average factors of 0.7 and 0.5 were calculated for the transfer of the total residue of BYI08330 from beans with pod into washed and cooked beans, respectively

. Transfer factors are given in Table B.7.7.2.2.7-5.

Table B.7.7.2.2.7-5: Transfer factors for the tota l residue of BYI08330 into processed commodities related to Climbing French bean with pod:

Transfer Factors for Total Residue of BYI08330 Sample material R 2004 0172/8 R 2004 0173/6 R 2004 0174/4 R 2004 01 75/2 mean Bean with pod, washed 0.7 0.7 0.7 0.8 0.7 Washings 0.2 * 0.5 * 0.1 0.1 0.2 Bean with pod, cooked 0.3 0.6 0.5 0.5 0.5 Cooking water 0.3 0.5 * 0.2 0.3 0.3

* For calculation of the transfer factors, residues below the LOQ were set at the LOQ.



### Conclusion: As the average transfer factors resulting from Clim bing French bean processing into bean, cooked; bean with pod, washed were <1.0, no concentration of BYI08330 is to be expected in these commodities during processing.

B.7.7.2.2.8 Beer

Reference: Determination of the residues of BYI 08330 in/on ho p cone green for processing and the processed fractions (cone kiln-d ried, beer, hops draff, brewer ́s yeast, brewer ́s malt)after spraying of BYI 08330 (OG100) in the field in northern France and Germany Author(s), year: Schöning R., Billian P., Wolters, A.; 2006 Report/Doc. number: RA-3036/04, including trials no . R 2004 0148/5, R 2004 0149/3, R 2004 0150/7, R 2004 0151/5 M-265067-01-1 Guideline(s): EU Council Directive 91/414/EEC of Ju ly15, 1991, Annex II, part A, section 6 and Annex III, part A, section 8: Residues in or on tr eated products, food and feed GLP: Yes. Deviations: None. Validity: The study is considered acceptable. The purpose of the presented study was to determine the transfer of BYI 08330 and its metabolites (BYI08330-enol, BYI08330-ketohydroxy, BYI08330-mono -hydroxy and BYI08330-enol-Glc) from green hop cones via kiln-dried hop cones into hop processed c ommodities (beer) and by-products obtained during brewing processing (hops draff; brewer’s yeast; bre wer’s malt).

Material and Method: Hop cone samples from four field trials that were p erformed in Northern France and Germany as part of study RA-2036/04 with BYI 08330 (100 OD) were proce ssed. Representative samples of the raw agricultura l commodity (hop, cone green), processed commodities and processing by-products were analysed for residues of BYI 08330 and its metabolites. Information about the treated plots is given in Tab le B.7.7.2.2.8-1.

### - 185 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.7.2.2.8-1: Application Data Summary in/o n hops in Northern Europe:

Country Trial No. Number Formulation Kg a.s./ha Kg a.s./hL Growth stage

BBCH

Northern France R 2004 0148/5 2 OD 100 0.1750 0.00729 - 0.00795 65-75

Germany R 2004 0149/3 2 OD 100 0.1620 - 0.1750 0.00700 - 0.00702 68-75

Germany R 2004 0150/7 2 OD 100 0.1750 0.00700 71-77

Northern France R 2004 0151/5 2 OD 100 0.1750 0.00795 75-81



### All samples were stored in a freezer at -18°C or be low until preparation of the examination samples. F or the preparation of examination samples of raw agricultu ral commodity, processed commodities and processing by-products, the deep-frozen samples were shredded with dry ice in a cutter. Representative parts of t he shredded samples were stored at -18°C or below unti l analysis.

Processing Procedures: Hop samples (cone, green) for processing were taken from the treated plots on day 14 (trials R 2004 14 8/5, R 2004 0149/3 and R 2004 0150/7) and on day 15 (tri al R 2004 0151/5) after the last application, respectively. Green cone samples were dried in a dr ying oven until approx. 10 % remaining moisture to get cone, kiln-dried samples for processing. The kiln-d ried hop cones were processed simulating industrial procedures (see Table B.7.7.2.2.8-2), whereby the d egradation of the active ingredients was kept to a minimum (worst case situation). This was achieved b y a minimum of processing steps. The process comprised the following fractions : - Hops draff (drip dried cones) - Brewing malt - Brewer ́s yeast - Beer The processing of hops to beer included the followi ng procedures : - grinding of malt - mashing - lautering - boiling of wort and addition of hops - brewing malt separation - fermentation - cold storage and maturation - filtration and bottling

Table B.7.7.2.2.8-2: Preparation of processed frac tions: Grinding Brewing malt was ground by one passage through the m alt-mill. The grist was not fractionated

after grinding. An aliquot of the brewing malt was taken as a specimen. Mashing The grist was mashed into water which was heated to approx. 50°C in the mashing tub. While

the grist was added and during the whole mashing pr ocedure the mixture was stirred continuously. When all the grist was mashed in, the vessel was heated After the mashing procedure the mash was drained off into the heated lauter tub. Lautering The wort was separated from spent grain in the laut er tub by filtration. The remainder was

washed with two portions of sparging water. The lea chates were transferred into the kettle. Dried Cone Addition and Wort Boiling A calculated weight of dried cones was placed into a cotton bag. The cotton bag was closed

and immersed into the wort which was subsequently h eated up to boil and kept boiling. An aliquot of the hops (drip dry) was taken as a specimen.

### - 186 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Hot Trub Separation After completion of the boiling, the hot wort was dr ained into the whirlpool and the trub material

was separated by applying the whirlpool technique: Using the tangential inlet, the wort was brought into rotation. The rotation caused the trub material to settle on the middle of the bottom of the vessel. The cleared wort was pumped through the cooling system into the cooled fermentation vessel. The complete amount of the tru b (flocs) suspended in wort was weighed. The cleared wort was pumped into the fermentation v essel. The wort was cooled down by incubating the keg in a water bath. Fermentation Yeast suspended in water was added and the wort was aerated. The fermentation process was

allowed to progress under darkened conditions in th e closed fermentation vessel. Due to the carbon dioxide produced by the yeast during ferment ation, a slight pressure was built up in the vessel. This procedure is called pressure fermentat ion and represents the most common fermentation procedure in the brewing industry. Afte r 7 to 13 days the yeast had settled at the bottom of the vessel and the fermentation was compl ete. The green beer was drained off through the “bottom valve“and forced into a storage container by means of carbon dioxide. The yeast suspension remained in the keg and was remove d later through the "side valve" and the entire amount was weighed and frozen. The yeast was separated after de-frosting of the suspension by means of centrifugation. The centrifuged yeast was taken as a specimen for residue analysis. Cold Storage The container with the green beer was placed into a chamber of the cooling box set to a

temperature of approx. 0 to - 1°C. The green beer r emained there for a period of 8 to 15 days. Filtration At the end of the brewing process, the beer was clar ified by filtration in a filtration apparatus.

The beer was added, mixed with the filter aids and the slurry was filtered using a horizontal candle filter. The first running was discarded. Bottling Immediately after filtering, the beer was filled in to bottles through a spiral of stainless steel

tubing. The beer was forced out of the reservoir us ing carbon dioxide from a cylinder. Finally, the bottles were capped with crown caps using a cro wner. An aliquot of the beer was taken as a specimen.



### Storage period for samples : The storage period of deep-frozen samples ranged between 67 and 358 days.

Residues of BYI 08330 and its metabolites BYI08330- enol, BYI08330-ketohydroxy, BYI08330-mono-hydroxy and BYI08330-enol-Glc in/on hop (cone, green; cone, kilndried, beer; hops draff; brewer’s yeast, brewe r’s malt) were determined by HPLC-ESIMS/ MS according t o method 00857.

Cone, green; Cone, kiln-dried; Hops draff: The Limit of Quantitation (LOQ) , defined as the lowest validated fortification lev el (calculated as BYI 08330 equivalents), was 0.10 mg/kg (BYI 08330), 0.12 mg/k g (BYI08330-enol, BYI08330-ketohydroxy, BYI08330- mono-hydroxy) and 0.08 mg/kg (BYI08330-enol-Glc) fo r hop (cone, green; cone, kiln-dried; hops draff). The LOQ for the total residue of BYI 08330 (sum of sing le analyte residues, each calculated as BYI 08330 equivalents) was calculated as 0.54 mg/kg for hop (cone, green; cone, kilndried; hops draff)

.

Beer; Brewer’s Yeast; Brewer’s Malt: The Limit of Quantitation (LOQ) , defined as the lowest validated fortification lev el (calculated as BYI 08330 equivalents), was 0.01 mg/kg (BYI 08330), 0.012 mg/ kg (BYI08330-enol, BYI08330-ketohydroxy, BYI08330- mono-hydroxy) and 0.008 mg/kg (BYI08330-enol-Glc) f or hop (beer; brewer’s yeast, brewer’s malt). The LOQ for the total residue of BYI 08330 (sum of sing le analyte residues, each calculated as BYI 08330 equivalents) was calculated as 0.054 mg/kg for hop (beer; brewer’s yeast; brewer’s malt).

Procedural recovery results are summarized in Table B.7.7.2.2.8-3.

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Table B.7.7.2.2.8-3: Recovery results (concurrent recoveries) for determination of BYI 08330 and its metabolites in hop cones, green and in processed co mmodities Sample Material Hop (cone green) Hop (cone kilndried)) Beer Brewer’s yeast Brewer’s yeast

Analyte Fortification levels *) Mean

Recovery [%±RDS] Fortification levels *) Mean

Recovery [%±RDS] Fortification levels Mean

Recovery [%±RDS] Fortification levels Mean

Recovery [%±RDS] Fortification levels Mean

Recovery [%±RDS] BYI 08330 0.1

5.0 83 ±16.4

(n=8) 0.1

5.0 86

±12.4 (n=11) 0.01

0.1 5.0 102

±13.7 (n=4) 0.01

0.1 5.0 93 ± 6.1

(n=7) 0.01

0.1 5.0 93 ± 4.7

(n=7)

BYI08330 -enol 0.1

5.0 78 ±11.0

(n=8) 0.1

5.0 85

±10.8 (n=11) 0.01

0.1 5.0 105 ±5.5

(n=4) 0.01

0.1 5.0 95 ± 8.2

(n=7) 0.01

0.1 5.0 95 ± 3.4

(n=7)

BYI08330-ketohydroxy 0.1

5.0 82 ± 9.2

(n=8) 0.1

5.0 84 ± 8.8

(n=11) 0.01

0.1 5.0 101 ±9.9

(n=4) 0.01

0.1 5.0 98 ± 7.2

(n=7) 0.01

0.1 5.0 95 ± 5.9

(n=7)

BYI08330

-monohydroxy 0.1

5.0 78 ±10.8

(n=8) 0.1

5.0 82 ± 7.9

(n=11) 0.01

0.1 5.0 99 ± 7.0

(n=4) 0.01

0.1 5.0 93 ±8.4

(n=7) 0.01

0.1 5.0 92 ± 4.4

(n=7)

BYI08330 -enol-Glc 0.1

5.0 78 ±10.4

(n=8) 0.1

5.0 80

±11.6 (n=11) 0.01

0.1 5.0 98 ± 9.6

(n=4) 0.01

0.1 5.0 95 ± 5.7

(n=7) 0.01

0.1 5.0 91 ± 5.6

(n=7)

*) levels refer to fortification with individual anal ytes (not calculated as BYI 08330 equivalents). 

### The mean of the recoveries were for all matrices an d for all fortification levels, within the acceptab le range of

70 – 110 %.

Findings: The total residue of BYI08330 in kiln-dried cones r anged between 1.5 and 4.2 mg/kg. The total residue in beer samples was below the LOQ of 0.055 mg/kg from each of four processing studies. The results are summarised in Table B.7.7.2.2.8-4.

Table B.7.7.2.2.8-4: Residues of BYI 08330 in hop cones, green and in processed commodities Residues [mg/kg] Country / Trial No. Portion

analysed PHI

[days] BYI 08330 BYI 08330- enol BYI

08330-ketohydroxy BYI

08330-

monohydroxy BYI

08330- enol-Glc Total Res.

of BYI 08330 calc.

Northern France R 2004 0148/5 Cone green

cone kiln dried beer hops draff brewer’s yeast brewer’s malt 14 0.17 0.63 <0.01 <0.1 <0.01 <0.01 <0.12

0.18 <0.012 <0.12 0.017 <0.012 <0.12

0.30 <0.012 <0.12 0.012 <0.012 0.012

<0.012 <0.012 <0.012 0.012 0.13

0.41 <0.008 <0.08 <0.008 <0.008 <0.54

1.5 <0.054 <0.54 <0.054 <0.054 Germany R 2004 0149/3 Cone green

cone kiln dried beer hops draff brewer’s yeast 14 0.27 0.56 <0.01 <0.1 <0.01 <0.12

0.25 0.016 <0.12 0.076 0.17

0.39 0.012 <0.12 0.014 <0.12

<0.12 <0.012 <0.12 <0.012 0.21

0.50 0.008 <0.08 0.008 0.77

1.7 <0.054 <0.54 0.098 Germany R 2004 0150/7 Cone green

cone kiln dried beer hops draff brewer’s yeast 14 0.19 1.1 <0.01 <0.1 <0.01 <0.12

0.75 0.016 <0.12 0.062 0.14

0.75 0.012 <0.12 0.012 <0.12

<0.12 <0.012 <0.12 <0.012 0.26

1.3 0.008 <0.08 0.008 0.72

3.9 <0.054 <0.54 0.082 Northern France R 2004 0151/5 Cone green

cone kiln dried beer hops draff brewer’s yeast 14 0.63 2.6 <0.01 <0.1 <0.01 <0.12

0.32 0.023 <0.12 0.067 0.19

0.72 0.012 <0.12 0.012 <0.12

<0.12 <0.012 <0.12 <0.012 0.14

0.58 0.008 <0.08 0.008 1.1

4.2 <0.054 <0.54 0.087

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Based on the residue levels in the treated processi ng products transfer factors were calculated. The t ransfer factors for the processing products are calculated according to the following equation:

Transfer Factor = Residue concentration in the proc essed product [mg/kg] / Residue concentration in th e RAC [mg/kg]

For calculation of the transfer factors for the tot al residue in processed commodities total residues of below the LOQ, were set to the respective LOQ of 0.054 mg /kg (beer, brewer ́s yeast) or 0.54 mg/kg (hops draf f). An average factor of below 0.02 was calculated for the transfer of the total residue of BYI08330 from dried hop cones into beer. The average factor for the tra nsfer of the total residue into hops draff is below 0.24 and into brewer’s yeast is below 0.04. Transfer factors are given in Table B.7.7.2.2.8-5.

Table B.7.7.2.2.8-5: Transfer factors for the tota l residue of BYI08330 into processed commodities related to kiln-dried cones

Transfer Factors for Total Residue of BYI08330 Sample material R 2004 0148/5 R 2004 0149/3 R 2004 0150/7 R 2004 01 51/5 mean

Beer <0.04*. <0.03* <0.01* <0.01* <0.02 Hops draff <0.36*. <0.32* <0.14* <0.13* <0.24 Brewer’s yeast <0.04*. 0.06 0.02 0.02 <0.04

* Residues in processed RAC were below LOQ. For cal culation of the transfer factor the residues in the processed RAC were set at the LOQ of 0.054 mg/kg (brewer`s yeast, beer ) or 0.54 mg/kg (hops draff).



### Conclusion: As the average transfer factors resulting from hops (kiln dried cones) processing into beer, hops draf f and brewer’s yeast were <1.0, no concentration of BYI08 330 is to be expected in these commodities during processing.

B.7.8 Livestock feeding studies (Annex IIA 6.4; Ann ex IIIA 8.4)

Relevant for EU: Estimation of the dietary burden for livestock anim als: Residues of Spirotetramat in animal feed might occu r after treatment of head and leafy brassica, when kale or/and cabbage are fed to livestock. Residues might also be found in animal feed after treatment of ci trus or pome fruit, when citrus dried pulp or apple wet pom ace are fed to cattle. Intake calculations for chic ken as well as for dairy and beef cattle were made taking into account the highest residue (see Tables B.7.9- 1 to B.7.9-3): Table B.7.8-1: Intake calculations* for chicken : Maximum daily intake of 0.12 kg dry matter for 1. 9 kg bodyweight:

Actual

crop Max. percentage

of actual crop in diet per day Intake of dry

matter from actual crop [kg/animal/day] % of

dry

matter

in

actual

crop Intake of fresh

material [kg/animal/day] Residue

in actual

crop (fresh material) [mg/kg] Residue intake

[mg/animal/day] Residue

intake [mg/kg bw/day] Dietary

burden [mg/kg diet]

kale 5 0.006 14 0.043 0.765 0.03279 0.0173 0.273

* according to the Document 7031/VI/95/rev.4 (22.7. 1996), Appendix G, Livestock Feeding Studies

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Although the dietary burden exceeds the trigger of 0.1 mg a.s./kg feed, no residues of spirotetramat a bove 0.01 mg/kg are expected in edible tissues or eggs w ith respect to the metabolism study in laying hens. Therefore no feeding study in poultry was required. Table B.7.8-2: Intake calculations* for beef catt le : Maximum daily intake of 15 kg dry matter for 350 kg bodyweight:

Actual

crop Max.

percentage

of actual crop in diet per day Intake of dry

matter from actual crop [kg/animal/day] % of

dry

matter

in

actual

crop Intake of fresh

material [kg/animal/day] Residue

in actual

crop (fresh material) [mg/kg] Residue intake

[mg/animal/day] Residue

intake [mg/kg bw/day] Dietary

burden [mg/kg diet]

kale 35 5.25 14 37.5 0.765 28.69 0.082 1.91

Apple

wet

pomace 30 4.5 23 19.6 0.28 ** 5.48 0.016 0.37

* according to the Document 7031/VI/95/rev.4 (22.7. 1996), Appendix G, Livestock Feeding Studies ** STMR (apples) of the Southern trials (0.113 mg/k g) x processing factor 2.5



### Table B.7.8-3: Intake calculations* for dairy catt le : Maximum daily intake of 20 kg dry matter for 550 kg bodyweight:

Actual

crop Max.

percentage

of actual crop in diet per day Intake of dry

matter from actual crop [kg/animal/day] % of

dry

matter

in

actual

crop Intake of fresh

material [kg/animal/day] Residue

in actual

crop (fresh material) [mg/kg] Residue intake

[mg/animal/day] Residue

intake [mg/kg bw/day] Dietary

burden [mg/kg diet]

kale 35 7 14 50.00 0.765 38.25 0.07 1.91

Apple

wet

pomace 10 2 23 8.7 0.28 2.43 0.004 0.12

* according to the Document 7031/VI/95/rev.4 (22.7. 1996), Appendix G, Livestock Feeding Studies ** STMR (apples) of the Southern trials (0.113 mg/k g) x processing factor 2.5



### Kale and fruit pomace belong to the same group of f eeding stuff (Group I, green forage). As it is poin ted out in the tables above, the relevant contributor to th e dietary burden is kale: In consequence of the dietary burden of 1.9 mg a.i. /kg feed (dry weight basis), a feeding study in dai ry cattle was designed to quantify the residues found in tiss ues and milk from dairy cows following oral adminis tration of spirotetramat:

Reference: BYI08330 150 OD - Magnitude of the residue lactatin g cows Author(s), year: Mackie, S. J. W. Report/Doc. number: Report No.: RAFNX014, Edition Number: M-276834-01-1 Guideline(s): PMRA Directive 98-02; DACO 7.5.1/EPA OPPTS 860.1480 GLP: Yes. Deviations: None. Validity: The study is considered acceptable.

### - 190 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Material and methods:

Spirotetramat was administered via capsule to ten l actating Holstein dairy cows for 29 consecutive day s. The target dose rates (based on feed dry weight) we re 0 mg/kg feed/day (control), 3.0 mg/kg feed/day, 9.0 mg/kg feed/day, or 30 mg/kg feed/day. Milk was col lected twice daily during the dosing period. Milk samples from the 30-mg/kg dose group were analyzed for spir otetramat residue on study days 0, 1, 3, 7, 10, 14, 17, 21, 24, 26, and 28. Additionally, a portion of the 26-day milk sample from the 30-mg/kg dose group wa s separated into milk fat (cream) and skim milk, and each was analyzed. On day 29, the animals were sacrificed and liver, kidney, composite muscle, and composite fat were collected for analysis. The ti ssue and milk samples in this study were analyzed within 19 days of collection; therefore, freezer storage stab ility studies on beef tissue and milk matrices were not r equired.

The total spirotetramat residue in tissue and milk samples was quantitated by high-performance liquid chromatography-electrospray ionization/tandem mass spectrometry (LC-MS/MS) using isotopically labeled internal standards. The individual analyte residue s of spirotetramat (parent) and the metabolites BYI 08330- enol, and BYI 08330-enol-glucuronide (hereinafter r eferred to as BYI 08330-enol-GA), were summed to gi ve a total spirotetramat residue in parent equivalents . The limit of quantitation (LOQ) was 0.005 mg/kg f or each analyte in milk matrices and was 0.010 mg/kg for ea ch analyte in the tissue matrices.

Findings :

Total spirotetramat residue in the milk samples fro m the 30-mg/kg feeding level were at or below the L OQ (0.005 mg/kg) in all cows throughout the study with the exception of a maximum residue of 0.006 mg/kg in one cow on study day 10. Residues of parent equival ents did not concentrate in samples of skim milk or milk fat separated from whole milk.

Table B.7.8-4: Residue Data in Milk from Lactating Cattle Feeding Study with Spirotetramat Matrix/Collection Time Feeding Level (mg/kg) Total Residues (mg/kg) Milk/Day 0 30 < 0.005, < 0.005, < 0.005 Milk/Day 1 30 < 0.005, < 0.005, < 0.005 Milk/Day 3 30 < 0.005, < 0.005, < 0.005 Milk/Day 7 30 < 0.005, < 0.005, < 0.005 Milk/Day 10 30 0.005, 0.006, < 0.005 Milk/Day 14 30 0.005, < 0.005, < 0.005 Milk/Day 17 30 < 0.005, 0.005, < 0.005 Milk/Day 21 30 0.005, 0.005, < 0.005 Milk/Day 24 30 < 0.005, < 0.005, < 0.005 Milk/Day 26 30 < 0.005, < 0.005, < 0.005 Milk fat/Day 26 30 < 0.005, < 0.005, < 0.005 Skim Milk/Day 26 30 < 0.005, < 0.005, < 0.005 Milk/Day 28 30 < 0.005, < 0.005, < 0.005



### A low tissue burden was observed, with the highest residues found in kidney at the three dosing levels (0.022 mg/kg, 0.075 mg/kg and 0.274 mg/kg, respecti vely). Despite the variability in the amount of to tal spirotetramat residues, there appeared to be a line ar relationship with the dosing levels in kidney, f at and liver tissues at the three feeding levels. At the 3-mg/kg dosing level, average residues of spirotetr amat equivalents were less than the LOQ (0.01 mg/kg) in fat, muscle and liver. The total average spirotetr amat residues were <0.010 mg/kg (muscle), 0.012 mg/kg (f at), and 0.016 mg/kg (liver) at the 9-mg/kg dosing level. At the 30-mg/kg dosing level, the total average spi rotetramat residues in muscle, fat and liver were 0 .012 mg/kg, 0.028 mg/kg, and 0.040 mg/kg, respectively.

### - 191 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Table B.7.8-5: Summary of Residue Data from Lactati ng Cattle Feeding Study with Spirotetramat. Total Spirotetramat Residue Levels (ppm) Matrix Feeding Level (mg/kg) n Min. Max. Median Mean) Std. Dev.

Milk 30 30 < 0.005 0.006 < 0.005 < 0.005 0.0006

Milk fat 30 3 < 0.005 < 0.005 < 0.005 < 0.005 - Skim Milk 30 3 < 0.005 < 0.005 < 0.005 < 0.005 -

Fat 3 3 < 0.010 < 0.010 < 0.010 < 0.010 -

Fat 9 3 < 0.010 0.017 < 0.010 0.0123 0.004

Fat 30 3 < 0.010 0.038 0.037 0.0283 0.016 Kidney 3 3 0.021 0.025 0.021 0.022 0.002 Kidney 9 3 0.051 0.103 0.070 0.075 0.026 Kidney 30 3 0.184 0.437 0.200 0.274 0.142

Muscle 3 3 < 0.010 < 0.010 < 0.010 < 0.010 -

Muscle 9 3 < 0.010 < 0.010 < 0.010 < 0.010 -

Muscle 30 3 < 0.010 0.016 0.011 0.012 0.003

Liver 3 3 < 0.010 < 0.010 < 0.010 < 0.010 -

Liver 9 3 0.013 0.018 0.016 0.016 0.003

Liver 30 3 0.031 0.057 0.032 0.040 0.015



### Conclusion: Relevant for PMRA (Canada) and US EPA : An adequate dairy cow feeding study has been submit ted; this study is acceptable for determining MRL levels for livestock commodities. Based on the sub mitted data, MRLs expressed as spirotetramat and th e metabolite BYI 08330-enol are required for some for livestock commodities. The potential for secondar y transfer of spirotetramat residues of concern in me at, milk, and eggs exists because there are livesto ck feedstuffs associated with the proposed uses on app les, citrus, potatoes, and almonds.As none of the proposed target crops are considered as a commodity for poultry feed, data depicting residues in layin g hens are not required. Expected secondary residues in meat and milk : The anticipated secondary residues in cattle matric es were estimated using transfer coefficient factor s calculated from the maximum residues of spirotetram at and the metabolites observed at the 30-mg/kg dos e level. The transfer coefficients (calculated as res idue-level-to-feed ratios) are presented in the tab le below. The transfer coefficient for each matrix was then u sed to calculate the expected secondary residues by multiplying the transfer coefficient by the calcula ted dietary burden.

Table B.7.8-6: Residue-Level-to-Feed Ratios (Transf er Coefficients) in Dairy Cattle Milk and Tissues1

Matrix Maximum Residue

(ppm) Feeding Level, ppm Transfer Coefficient

Milk 0.011 0.00037 Fat 0.038 0.0013 Muscle 0.016 0.00053 Kidney 0.437 0.0146 Liver 0.057 30

0.0019

1 Calculated from the maximum residues observed at the dose level closest to the RBDB divided by the dos e level.



### Table B.7.8-7: Secondary Residues and Proposed MRLs :

Matrix Dietary burden

(ppm) Secondary Residues (ppm) 1 Proposed MRL 2 (ppm)

Milk 1.0 0.00037 0.01

Fat 0.0016 0.02 Kidney 1.2

0.018 0.02

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Matrix Dietary burden

(ppm) Secondary Residues (ppm) 1 Proposed MRL 2 (ppm)

Muscle 0.00064 0.02

Liver 0.0023 0.02

1 Calculated from dietary burden x transfer coeffic ient from previous table.

2 LOQ-level MRL in order to harmonize with Canada.



### Relevant for EU : As the lowest dose rate of the feeding study was 3. 0 mg a.i./kg dry feed instead of the expected highe st intake of 1.9 mg a.i./kg dry feed, extrapolation is not possible. Therefore the following transfer fac tors for kidney were calculated, as only kidney showed resid ues above the LOQ in the lowest dose group:

Table B.7.8-8: Transfer factors for kidney (concent ration mg a.i./kg tissue / concentration mg a.i./kg feed)

Mean concentration found in kidney [mg/kg] Dose group [mg/kg] Transfer factor Calculated concentration in kidney for dietary burden of 1.9 mg a.i./kg 0.022 3 0.0073 0.014 mg/kg 0.075 10 0.0075 0.014 mg/kg



### For these results a MRL of 0.02 mg/kg is proposed f or bovine, sheep, goat and swine kidney. The LOQ of 0.01 mg/kg refers to BYI08330-enol only, calculated and expressed as BYI08330 parent equivalents; as f or the time being no analytical monitoring method is a vailable for parent spirotetramat. However, the par ent compound was not found in any livestock tissue. Conclusion: Basing on the results of the livestock feeding stud y, a MRL of 0.02 mg/kg is proposed for bovine, shee p, goat and swine kidney. For other edible tissues no MRL i s required (LOQ at 0.01 mg/kg), also not for milk ( LOQ at 0.005 mg/kg).

B.7.9 Residues in succeeding crops or rotational cr ops (Annex IIA 6.6; Annex IIIA 8.6)

B.7.9.1 Confined rotational crop study using radiol abelled material

Reference: Metabolism of [Azaspirodecenyl-3-14C]BYI 08330 in C onfined Rotational Crops. Amendment No.1 of September 8, 2006. Author(s), year: Sur, R., Spiegel, K. (2006) Report/Doc. number: Report No.: MEF-05/288, Edition Number: M-269589-02-2 Guideline(s): PMRA Directive 98-02; DACO 7.4.3/EPA OPPTS 860.1850 GLP: Yes. Deviations: No. Validity: Yes.

Material and methods:

The metabolism in rotational crops (spring wheat, S wiss chard and turnips) was investigated following spray application of [azaspirodecenyl-3- 14 

### C]-spirotetramat onto bare soil (day 0) at an appli cation rate of 406 g a.i./ha (0.36 lbs. a.i./A). Crops were sown at day 30, day 135, and day 260. Representative immature and mature plant samples were analysed.

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The radioactivity in the extracts of all RACs obtai ned after conventional extraction was partitioned w ith dichloromethane (DCM), yielding a DCM phase and an aqueous phase. The phases were analysed (if the TRR exceeded 0.01 mg-equiv./kg) and the metabolites were quantified by high-performance liquid chromatography (HPLC). Identification of metabolit es was performed by spectroscopic methods (HPLCmass spectrometry (MS)/MS, Fourier Transform (FT)-M S and 1 

### H-nuclear-magnetic resonance (NMR) spectroscopy) or by HPLC and thin-layer chromatogra phy (TLC) co-chromatography using authentic reference compounds.

Since a major part of the residues were represented by conjugates, plant extracts were subjected to ac id hydrolysis to cleave the conjugates and to simplify the metabolic profiles for analysis of residues. BYI 08330-desmethyl-di-hydroxy, BYI 08330-ketohydroxy-a lcohol, and BYI 08330-desmethyl-ketohydroxy were identified as the major constituents of the residue s after hydrolysis.

Findings :

Sufficient data were available to support the stora ge intervals of the samples of all crops in this st udy. Storage stability data (reanalysis of extracts, re- extraction of stored samples over time) showed that metabolite pattern, as well as the proportions of m etabolites remained stable for at least 11 months w hen stored at ≤-18 °C.

The total radioactive residues (TRRs) were highest in wheat straw of the 30-day rotation (0.998 mgequiv./kg) followed by wheat hay (0.384 mg-equiv./k g), turnip leaves (0.123 mg-equiv./kg), Swiss chard (0.078 mg-equiv./kg), wheat grain (0.026 mg-equiv./ kg), wheat forage (0.024 mg-equiv./kg), and turnip roots (0.021 mg-equiv./kg). A significant decline of the TRR from the 30-day to the 260-day rotation was ob served in all raw agricultural commodities (RACs). In the 260-day rotation, only wheat hay and wheat straw s howed residues above 0.01 mg-equiv./kg. The lowest resid ues were generally detected in the edible matrices of wheat grain and turnip roots, followed by Swiss cha rd.

The majority of the radioactivity was extracted con ventionally using acetonitrile (ACN)/water and ACN as solvents, except for samples of wheat grain. Appro ximately 83 to 97% of the TRR in the 30-day rotatio n crops, and 72 to 93% of the TRR in the 135-day rota tion crops were extracted (grain excluded). In the 260- day rotation, only wheat straw and wheat hay (contained TRRs >0.01 mg-equiv./kg) were extracted, releasing 81% and 87% of the TRRs, respectively. F or wheat grain (30-day and 135-day rotation) and wh eat straw (30-day rotation), exhaustive extractions of post-extraction solids (PES 1) were conducted follo wing the conventional extraction steps. The PES 1 of wheat grain containing 50-79% of the TRR was further trea ted with enzyme diastase and 45-67% of the TRR was rele ased. The PES 1 of wheat straw containing 8% of the TRR was microwave extracted with ACN/water at 1 20°C; and, 4% of the TRR was further released.

Summaries of characterization and identification of radioactive residues in the different plantback in tervals are given in Tables B.7.9.1-1, B.7.9.1-2 and B.7.9. 1-3.- 194 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Table B.7.9.1-1: Summary of Characterization and Identification of Radioactive Residues in 30-day PBIRotational Crop Matrices Following Applicationof Radiolabeled Spirotetramat at 406 g a.i./ha.wheat forage wheat hay wheat straw wheat grain Swiss chard turnip leaves turnip rootsTRR0.024 mg-equiv./kg0.384 mg-equiv./kg0.998 mg-equiv./kg0.026 mg-equiv./kg0.078 mg-equiv./kg0.123 mg-equiv./kg0.021 mg-equiv./kgMetabolite Fraction (BYI 08330-) %TRRmgequiv./kg%TRRmgequiv./kg%TRRmgequiv./kg%TRRmgequiv./kg%TRRmgequiv./kg%TRRmgequiv./kg%TRRmgequiv./kgdesmethyl-di-hydroxy-Glc 2.6 0.001 6.9 0.027 12.7 0.127 4.5 0.001 3.8 0.003 4.3 0.005 -- --enol-Glc -- -- 1.3 0.005 4.1 0.041 -- -- -- -- -- -- -- --desmethyl-di-hydroxy -- -- 1.2 0.005 2.5 0.025 2.30.001 -- -- 1.9 0.002 -- --desmethyl-di-hydroxy-Glc-MA -- -- 4.0 0.015 6.0 0.060 1.3 <0.001 5.3 0.004 3.7 0.005 6.0 0.001ketohydroxy-alcohol-Glc 2.7 0.001 4.7 0.018 5.8 0.058 1.4 <0.001 -- -- 5.3 0.007 -- --desmethyl-ketohydroxy-Glc (I1) -- -- 10.6 0.041 8.70.087 0.8 <0.001 15.2 0.012 -- -- -- --desmethyl-ketohydroxy-Glc (I2) 31.7 0.008 7.2 0.0284.4 0.044 0.8 <0.001 9.2 0.007 5.2 0.006 -- --desmethyl-enol-alcohol 1.6 <0.001 0.8 0.003 0.5 0.005 0.5 <0.001 2.2 0.002 0.3 <0.001 2.8 0.001di-hydroxy 5.0 0.001 5.3 0.020 5.7 0.057 2.0 0.0018.1 0.006 1.5 0.002 7.7 0.002ketohydroxy-alcohol -- -- 6.9 0.027 1.8 0.018 0.8 <0.001 1.6 0.001 6.8 0.008 -- --desmethyl-ketohydroxy-Glc-MA (I1) 1.8 <0.001 11.5 0.044 8.8 0.088 1.5 <0.001 -- -- -- -- -- --desmethyl-ketohydroxy-Glc-MA (I2) 2.2 0.001 4.0 0.016 3.8 0.038 1.4 <0.001 -- -- 4.8 0.006 -- --desmethyl-ketohydroxy 2.3 0.001 0.6 0.002 2.2 0.022-- -- 0.9 0.001 0.3 <0.001 4.2 0.001Ketohydroxy 31.4 0.008 8.4 0.032 3.1 0.031 -- -- 17.4 0.014 2.6 0.003 29.5 0.006Enol-- -- -- -- -- -- 2.9 0.001 -- -- -- -- -- --Total identified 81.3 0.020 73.5 0.282 70.1 0.700 20.1 0.005 63.7 0.050 36.7 0.045 50.1 0.011Total characterized 5.3 0.001 20.3 0.078 26.3 0.26230.0 0.008 27.5 0.021 60.4 0.074 32.5 0.007Total extractable (conventional) 86.7 0.021 93.6 0.360 92.1 0.919 50.1 0.013 91.3 0.071 97.1 0.120 82.6 0.017Total bound (solids 1) 13.3 0.003 6.4 0.025 7.9 0.079 49.9 0.013 8.7 0.007 2.9 0.004 17.4 0.004Total extractable (exhaustive) -- -- -- -- 4.3 0.043 44.5 0.012 -- -- -- -- -- --Total bound (solids 2) -- -- -- -- 3.6 0.036 5.4 0.001 -- -- -- -- -- --Accountability 100.0 0.024 100.0 0.384 100.0 0.998100.0 0.026 100.0 0.078 100.0 0.123 100.0 0.021- 195 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Table B.7.9.1-2: Summary of Characterization and Identification of Radioactive Residues in 135-day PBIRotational Crop Matrices FollowingApplication of Radiolabeled Spirotetramat at 406 ga.i./ha.wheat forage wheat hay wheat straw wheat grain Swiss chard turnip leaves turnip rootsTRR0.021 mg-equiv./kg0.038 mg-equiv./kg0.097 mg-equiv./kg0.010 mg-equiv./kg0.012 mg-equiv./kg0.015 mg-equiv./kg0.003 mg-equiv./kgMetabolite Fraction (BYI 08330-) %TRRmgequiv./kg%TRRmgequiv./kg%TRRmgequiv./kg%TRRmgequiv./kg%TRRmgequiv./kg%TRRmgequiv./kg%TRRmgequiv./kgdesmethyl-di-hydroxy-Glc 18.3 0.004 14.0 0.005 9.20.009 4.5 0.001 5.5 0.001enol-Glc -- -- 1.7 0.001 1.9 0.002 -- -- -- --desmethyl-di-hydroxy -- -- -- -- 2.9 0.003 -- -- ----desmethyl-di-hydroxy-Glc-MA 9.1 0.002 11.5 0.004 5.8 0.006 3.5 <0.001 4.3 0.001ketohydroxy-alcohol-Glc -- -- 3.2 0.001 1.3 0.001 -- -- 2.6 <0.001desmethyl-ketohydroxy-Glc (I1) 8.7 0.002 6.5 0.0027.3 0.007 6.2 0.001 -- --desmethyl-ketohydroxy-Glc (2) 5.6 0.001 3.2 0.001 2.7 0.003 5.9 0.001 5.5 0.001desmethyl-enol-alcohol -- -- -- -- -- -- -- -- -- --di-hydroxy -- -- -- -- 10.6 0.010 16.8 0.002 -- --ketohydroxy-alcohol -- -- -- -- -- 3.8 <0.001 4.60.001desmethyl-ketohydroxy-Glc-MA (I1) 8.0 0.002 5.4 0.002 5.6 0.005 -- -- -- --desmethyl-ketohydroxy-Glc-MA (I2) 2.5 0.001 -- -- 2.0 0.002 -- -- -- --desmethyl-ketohydroxy -- -- -- -- 1.8 0.002 2.3 <0.001 3.5 0.001ketohydroxy -- -- -- -- 7.1 0.007 14.9 0.002 -- --enol-- -- -- -- -- -- -- -- --desmethyl-di-hydroxy-Glc -- -- -- -- -- --NA ---- -- -- --NA --Total identified 52.2 0.012 45.5 0.017 58.3 0.056 -- -- 57.8 0.007 26.0 0.004 -- --Total characterized *40.3 *0.009 *39.2 *0.015 29.70.029 -- -- 26.2 0.003 *59.7 *0.009 -- --Total extractable (conventional) 92.5 0.021 84.8 0.032 88.0 0.085 21.2 0.002 84.0 0.010 85.7 0.013 71.6 0.002Total bound (solids 1) 7.5 0.002 15.2 0.006 12.0 0.012 78.8 0.008 16.0 0.002 14.3 0.002 28.4 0.001Total extractable (exhaustive) -- -- -- -- -- -- 66.8 0.007 -- -- -- -- -- --Total bound (solids 2) -- -- -- -- -- -- 12.0 0.001-- -- -- -- -- --Accountability 100.0 0.021 100.0 0.038 100.0 0.097100.0 0.010 100.0 0.012 100.0 0.015 100.0 0.003Turnip roots were not extracted due to TRR <0.01 mg-equiv./kg. Wheat grain extracts were not analysed due to TRR <0.01 mg-equiv./kg* only the aqueous phase was analysed by HPLC (residue level >0.005 mg/kg); the compounds in the DCM phase were characterized due to their behaviourduring partitioning- 196 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Table B.7.9.1-3: Summary of Characterization and Identification of Radioactive Residues in 260-day PBIRotational Crop Matrices FollowingApplication of Radiolabeled Spirotetramat at 406 ga.i./ha.wheat forage wheat hay wheat straw wheat grain Swiss chard turnip leaves turnip rootsTRR0.009 mg-equiv./kg0.014 mg-equiv./kg0.036 mg-equiv./kg0.002 mg-equiv./kg0.006 mg-equiv./kg0.008 mg-equiv./kg0.002 mg-equiv./kgMetabolite Fraction (BYI 08330-) %TRRmgequiv./kg%TRRmgequiv./kg%TRRmgequiv./kg%TRRmgequiv./kg%TRRmgequiv./kg%TRRmgequiv./kg%TRRmgequiv./kgdesmethyl-di-hydroxy-Glc5.4 0.001 5.6 0.002enol-Glc-- -- -- --desmethyl-di-hydroxy-- -- -- --desmethyl-di-hydroxy-Glc-MA 9.7 0.001 4.4 0.002ketohydroxy-alcohol-Glc-- -- 4.9 0.002desmethyl-ketohydroxy-Glc (I1) 6.5 0.001 7.8 0.003desmethyl-ketohydroxy-Glc (2) 2.8 <0.001 4.8 0.002desmethyl-enol-alcohol-- -- -- --di-hydroxy-- -- 18.1 0.006ketohydroxy-alcohol-- -- -- --desmethyl-ketohydroxy-Glc-MA (I1) 4.2 0.001 7.3 0.003desmethyl-ketohydroxy-Glc-MA (I2) -- -- 7.6 0.003desmethyl-ketohydroxy-- -- -- --ketohydroxy-- -- 5.3 0.002enol-- -- -- --desmethyl-di-hydroxy-GlcNA ---- -- -- --NA -- NA -- NA -- NA --Total identified -- --28.7 0.004 65.9 0.024-- -- -- -- -- -- -- --Total characterized -- --*52.2 *0.007 21.30.008 -- -- -- -- -- -- -- --Total extractable (conventional) -- -- 80.8 0.011 87.3 0.031 -- -- -- -- -- -- -- --Total bound (solids 1) -- -- 19.2 0.003 12.7 0.005-- -- -- -- -- -- -- --Accountability1100.0 0.009 100.0 0.014 100.0 0.036 100.0 0.002 100.0 0.006 100.0 0.008 100.0 0.002Wheat hay, wheat grain, Swiss chard, turnip leavesand turnip roots were not extracted due to low TRR(<0.01 ppm)* only the aqueous phase was analysed by HPLC (residue level >0.005 ppm), the residues in the DCM phase were characterized due to their behavior duringpartitioning.

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Conclusion : Parent compound spirotetramat was not detected in a ny of the samples. Major metabolites (>10% of the TRR) in the 30-day and 135-day rotation were: BYI 08330-ketohydroxy, BYI 08330-desmethyl-ketohydroxyGlc (two isomers), BYI 08330-desmethyl-ketohydroxy- Glc-MA (two isomers), BYI 08330-desmethyldihydroxy-Glc, BYI 08330-desmethyl-di-hydroxy-Glc-M A, and BYI 08330-di-hydroxy. Other identified metabolites were of minor importance.

It appears that two major metabolic routes in rotat ional crops start with the soil metabolites BYI 083 30- ketohydroxy and BYI 08330-enol. The first metaboli c route proceeds by demethylation of the cyclohexyl ring or hydroxylation of one methyl group of the xylol r ing. Another metabolic route starts with the addit ion of water to the tetramic acid ring of BYI 08330-enol r esulting in the formation of BYI 08330-di-hydroxy, followed by the demethylation of the metabolite. Additional ly, hydroxylation of one methyl group of the xylol ring of BYI 08330-enol followed by demethylation of the cyc lohexyl ring results in BYI 08330-desmethyl-enolalcohol, which was detected in all matrices. Most of the metabolites were rapidly conjugated. Glucos ides and/or glucosyl malonic acid conjugates were detect ed for BYI 08330-enol, BYI 08330-desmethyl-di-hydro xy, BYI 08330-desmethyl-ketohydroxy and BYI 08330-ketoh ydroxy-alcohol. The percentage of conjugates increased from the 30-day to the 260-day rotation.

Overall conclusion with relevance for PMRA (Canada) and US EPA:: The submitted confined rotational crop study is ade quate to satisfy data requirements. The metabolism of spirotetramat in rotational crops appears to be con sistent with the pathway observed in the plant meta bolism studies. The following potential components of the residue definition were identified in the confined rotational crop study: BYI08330, BYI08330-ketohydroxy, and fre e and conjugated BYI08330-desmethyl-ketohydroxy, BYI08330-desmethyl-di-hydroxy and BYI-08330-ketohyd roxy-alcohol. None of these residues were found in the limited rotational crop field trials at a 30-da y PBI. Provided a 30-day PBI is specified on the s pirotetramat labels, residues in rotational crops are not of con cern for the risk assessment or for MRL setting.

Overall conclusion with relevance for EU: The results of the confined rotational crop study u sing radiolabelled material show that residues resu lting from the use of spirotetramat in primary crops migh t lead to residues >LOQ in rotational crops, which are not covered by the residue definition for plant matrice s. The crop rotation field studies conducted in 3 d ifferent regions in the USA (see point B.7.9.2) are consider ed acceptable as additional information to elucidat e, if the residue definition for primary crops has to be enla rged or not.

B.7.9.2 Crop rotation studies (field test)

Reference: BYI08330 100 OD – Magnitude of the Residue in Field Rotational Crops (Limited). Author(s), year: Lemke, V. (2006) Report/Doc. number: Report No.: RAFNY019, Edition Number: M-277284-01-1 Guideline(s): PMRA Directive 98-02; DACO 7.4.4/EPA OPPTS 860.1900 GLP: Yes. Deviations: None. Validity: The study is considered acceptable.

Material and methods:

The field rotational crop study was conducted in th ree sites in the US (FL, IL, CA) using BYI 08330 10 0 OD, an oil-dispersible formulation containing 100 g a.i ./L spirotetramat. BYI 08330 100 OD was applied, t wice at

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5-7 days apart, to a primary crop (leafy, Brassica , or fruiting vegetables) as foliar broadcast spray for a total rate of 0.172-0.180 kg a.i./ha (0.153-0.161 lb a.i. /A). After primary crops were removed, rotational crops (mustard greens, turnips and wheat) were planted at a 30-day plant-back interval (PBI) following the l ast application of BYI 08330 100 OD.

Residues of spirotetramat and BYI 08330-ketohydroxy were determined using analytical method 00857 with slight modification. Briefly, a 5.0 g aliquot of c rop matrix was extracted with 30 mL of acidic aceto nitrile (ACN)/water mixture (4/1, v/v) using Polytron blend er. After filtration and cleaning-up of the extrac t, the corresponding stable isotopically labelled internal standards were added. Afterwards, the solution wa s made up to volume, and subjected to high-pressure liquid chromatography with triple-stage quadrupole mass spectrometry (HPLC-MS/MS). The LOQ was 0.01 ppm ea ch for spirotetramat and BYI 08330-ketohydroxy.

Analytical method 00929 with slight modification wa s used to determine residues of BYI 08330-desmethyl -dihydroxy, BYI 08330-desmethyl-ketohydroxy and BYI 08 330-ketohydroxy-alcohol in rotational crops. Brief ly, a 2.5 g aliquot of crop matrix was soaked with 20 m L of ACN/water mixture (4/1, v/v) for 30 minutes an d blended using a high-speed blender. The extract wa s filtered through a 20 mL Varian Bond Elute reserv oir. The filtrate was diluted to 50 mL with ACN/water (1 /1, v/v) and concentrated to the aqueous remainder. The concentrated extract was hydrolyzed with 10 mL of 3 N HCl/water (1/1, v/v) at 100°C for 1 hour. After cooling, a mixture of isotopically labelled interna l standards was added, and the solution was made up to volume, purified through a 20-mL Varian Bond Elute reservoir. The purified solution was concentrated to near dryness, reconstituted with ACN/water (1/3, v/ v) and analyzed by HPLC-MS/MS. The LOQ is 0.02 ppm for each analyte.

Findings:

At maturity, samples of mustard greens, turnip (top s and roots), wheat (forage, hay, straw and grain) were collected and analyzed for residues of spirotetrama t, BYI 08330-ketohydroxy, BYI 08330-desmethylketohydroxy, BYI 08330-desmethyl-di-hydroxy and BYI 08330-ketohydroxy-alcohol. Adequate methodvalidation data were provided. No residues were de tected above the method’s limit of quantitation (LO Q) levels in any of the rotational crop matrices. Res idues of spirotetramat, BYI 08330-ketohydroxy were analyzed using analytical method 00857 with a LOQ o f 0.01 ppm for each analyte. Residues of BYI 08330

- desmethyl-ketohydroxy, BYI 08330-desmethy-di-hydrox y and BYI 08330-ketohydroxy-alcohol were analyzed using analytical method 00929 with a LOQ of 0.02 pp m for each analyte. The samples were analyzed after freezer storage of approximately 15 months. Freeze r storage stability information is available to sho w the residues of BYI 08330-ketohydroxy, BYI 08330-desmet hyl-ketohydroxy, BYI 08330-desmethyl-di-hydroxy and BYI 08330-ketohydroxy-alcohol are stable for at least 30 months in the subject crops.- 199 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Table B.7.9.2-1: Residues of spirotetramat equivalents in succeeding crops after application of BYI 08330 100 OD.Trial ID(City,State/Year)ZoneCrop/ Variety CommodityTotalRate,g a.i./ha(lb a.i./A)Harvest DAP1PBI2(days)Spirotetramat (mgequiv./kg)BYI 08330ketohydroxy(mgequiv./kg)desmethyldi-hydroxy(mgequiv./kg)desmethyl-ketohydroxy(mgequiv./kg)ketohydroxyalcohol(mg-equiv./kg)Molino, FL20043 Mustard greens/GiantSouthern Curledgreens(leaves)177.3(0.159)34 34 <0.01, <0.01 <0.01, <0.01 <0.02, <0.02 <0.02,<0.02<0.02, <0.02Seymour, Il20045 Mustard greens/GreenWavegreens(leaves)178.2(0.159)46 29 <0.01, <0.01 <0.01, <0.01 <0.02, <0.02 <0.02,<0.02<0.02, <0.02Molino, FL20043 Turnip/Purple Top WhiteGlobeTops(leaves)177.6(0.158)48 34 <0.01, <0.01 <0.01, <0.01 <0.02, <0.02 <0.02,<0.02<0.02, <0.02Seymour, Il20045 Turnip/Purple Top WhiteGlobeTops(leaves)179.2(0.160)59 29 <0.01, <0.01 <0.01, <0.01 <0.02, <0.02 <0.02,<0.02<0.02, <0.02Molino, FL20043 Turnip/Purple Top WhiteGlobeRoots 177.6(0.158)48 34 <0.01, <0.01 <0.01, <0.01 <0.02, <0.02 <0.02,<0.02<0.02, <0.02Seymour, Il20045 Turnip/Purple Top WhiteGlobeRoots 179.2(0.160)59 29 <0.01, <0.01 <0.01, <0.01 <0.02, <0.02 <0.02,<0.02<0.02, <0.02Molino, FL20043 Wheat, winter/Coker9125Forage 172.0(0.153)94 35 <0.01, <0.01 <0.01, <0.01 <0.02, <0.02 <0.02,<0.02<0.02, <0.02Seymour, Il20045 Wheat, winter/IL94-1653 Forage 180.4(0.161)185 29 <0.01, <0.01 <0.01, <0.01 <0.02, <0.02 <0.02,<0.02<0.02, <0.02Molino, FL20043 Wheat, winter/Coker9125Hay 172.0(0.153)154 25 <0.01, <0.01 <0.01, <0.01 <0.02, <0.02 <0.02,<0.02<0.02, <0.02Seymour, Il20045 Wheat, winter/IL94-1653 Hay 180.4(0.161)222 29 <0.01, <0.01 <0.01, <0.01 <0.02, <0.02 <0.02,<0.02<0.02, <0.02Molino, FL20043 Wheat, winter/Coker9125Grain 172.0(0.153)191 35 <0.01, <0.01 <0.01, <0.01 <0.02, <0.02 <0.02,<0.02<0.02, <0.02Seymour, Il20045 Wheat, winter/IL94-1653 Grain 180.4(0.161)257 29 <0.01, <0.01 <0.01, <0.01 <0.02, <0.02 <0.02,<0.02<0.02, <0.02Molino, FL20043 Wheat, winter/Coker9125Straw 172.0(0.153)191 35 <0.01, <0.01 <0.01, <0.01 <0.02, <0.02 <0.02,<0.02<0.02, <0.02Seymour, Il20045 Wheat, winter/IL94-1653 Straw 180.4(0.161)257 29 <0.01, <0.01 <0.01, <0.01 <0.02, <0.02 <0.02,<0.02<0.02, <0.02

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Conclusion: At PBI of 30 days, no residues of spirotetramat, BY I 08330-ketohydroxy, BYI 08330-desmethyl-ketohydrox y, BYI 08330-desmethyl-di-hydroxy and BYI 08330-ketohy droxy-alcohol were detected above their LOQ levels in rotational crops (mustard greens, turnips and wh eat).

Comment of RMS AT: The remark “limited” in the study title seems to gr ound on the following exceptions to the requirement s of EPA Good Laboratory Practice Standards: weather dat a, maintenance chemical applications, pesticide history data, irrigation records, cultural practice s, and field sample weights for the trials were not collected under GLP. Nevertheless the study is considered acc eptable by PMRA (Canada) and RMS AT.

B.7.9.3 Overall conclusion

The submitted field rotational crop data are adequa te to satisfy data requirements. The available dat a indicate that residues of the parent and the metabo lites (BYI 08330-ketohydroxy, BYI 08330-desmethylketohydroxy, BYI 08330-desmethyl-di-hydroxy and BYI 08330-ketohydroxy-alcohol) were each <0.020 ppm in/on all rotational crop matrices at a 30-day PBI. These data support a rotational crop restriction of 30 days for all non-labeled crops. Unless the applicant req uests PBIs shorter than 30 days, no additional data are required, and MRLs for inadvertent residues in/on r otational crops need not be established in conjunct ion with the currently proposed uses. Comments RMS Austria with relevance for EU: The expected residues in rotational crops are cover ed sufficiently by the residue definition for the e xpression of the MRL/monitoring and risk assessment for plant commodities (spirotetramat and the metabolites BYI 08330-enol, BYI 08330-ketohydroxy, BYI08330-enol-Gl c, and BYI 08330-mono-hydroxy), based on the outcome of the field trials in succeeding crops, wh ich are accepted by RMS Austria as additional infor mation.

B.7.10 Proposed pre-harvest intervals for envisaged uses, or withholding periods, in the case

of post harvest uses (Annex IIA 6.8; Annex IIIA 8.8 )

Table Table B.7.10-1: PHI proposed by the notifier after application of spirotetramat. Relevant for EU:

Crop Food/feed item PHI [days]

Citrus Food item 14 Lettuce (head and leafy) Food item 7 Pome fruit (apple, pear) Food item 21 Stone fruit (plum, sour and sweet cherry, peach, apricot, nectarine) Food item 21

Grapes Food item 14 Strawberries Food item 3 Onions Food item 7 Fruiting vegetables (tomatoes, peppers, aubergines) Food item 3

Cucurbit vegetables (cucmbers, courgettes, melon, watermelon) Food item 3

Flowering brassica (cauliflower, broccoli), head cabbage (red and white savoy) Food item 3

Brussel sprouts, kohlrabi Food item 3 Leafy brassica Food and feed item 3 Beans, green Food item 14 Hops Food item 14 

### Note: grey marked data are only intended for MRL se tting in the EU.

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B.7.11 Community MRL and MRLs in EU Member States ( Annex IIIA 11.2)

B.7.12 Proposed EU MRLs and justification for the a cceptability of those MRLs (Annex IIA

6.7; Annex IIIA 8.7)

Table B.7.12-1: Proposed MRLs for Food of plant ori gin

Commodity Proposed EU-MRLs according to the intended uses [mg/kg] 1) Comments

Citrus 1 Import tolerance (0.5 mg/kg based on EU-GAP) Lettuce 5 --- (No import tolerance. Intended for us e in NAFTA, but no residue data submitted.) Tree nuts 0.5 Import tolerance (no EU-GAP) Pome fruit 1 Import tolerance (0.3 mg/kg based on EU- GAP) Peach / Apricots 2 Import tolerance (1 mg/kg based on EU-GAP) Cherries 5 Import tolerance (1 mg/kg based on EU-GAP) Plums 2 Import tolerance (2 mg/kg also based on EU-GAP) Grapes 2 Import tolerance (1 mg/kg based on EU-GAP) Strawberries 1 --- Potatoes 0.5 Import tolerance (no EU-GAP) Onions 0.3 ---

Tomatoes 2 --- Peppers 2 Import tolerance (2 mg/kg also based on EU- GAP) Aubergines 2 Extrapolated from tomatoes. Cucumbers 0.2 Import tolerance (0.2 mg/kg also base d on EUGAP) Courgettes 0.2 Extrapolated from cucumbers. Cucurbits (inedible peel) 0.3 Import tolerance Flowering brassica 1 Import tolerance (1 mg/kg base d on EU-GAP) Brussel sprouts 0.3 --- Head cabbage 2 Import tolerance (0.5 mg/kg based on EU-GAP) Leafy brassica 10 Import tolerance (2 mg/kg based o n EU-GAP)

Kohlrabi 2 --- Green beans 2 --- Hops 20 Import tolerance (10 mg/kg based on EU-GAP)

1) Residues expressed in mg spirotetramat /kg



### B.7.12.1 Food of animal origin

Proposal relevant for EU: Basing on the results of the livestock feeding stud y, a MRL of 0.02 mg/kg is proposed for bovine, shee p, goat and swine kidney. For other edible tissues no MRL i s required (LOQ at 0.01 mg/kg), also not for milk ( LOQ at 0.005 mg/kg).

Table B.7.12.1-1: EU-MRLs Proposed by RMS for Food of animal origin

Commodity Proposed EU-MRLs according to the intended uses [mg/kg] 1) Comments

Kidney (bovine, goat, sheep, swine) 0.02 ---

1) Residues expressed in mg spirotetramat /kg

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Table B.7.12.1-2: MRLs Proposed by Canada for Food of animal origin

Commodity Proposed NAFTA-MRLs according to the intended uses [mg/kg] 1) Comments

Milk 0.01 --- Cattle, meat 0.02 --- Cattle, fat 0.02 --- Cattle, meat byproducts 0.02 --- Goat, meat 0.02 --- Goat, fat 0.02 --- Goat, meat byproducts 0.02 --- Sheep, meat 0.02 --- Sheep, fat 0.02 --- Sheep, meat byproducts 0.02 --- Horse, meat 0.02 --- Horse, fat 0.02 --- Horse, meat byproducts 0.02 ---

1) Residues expressed in mg spirotetramat /kg



### B.7.13 Proposed EU import tolerances and justificat ion for the acceptability of those

residues

Please refer to Annex III (the evaluation of the im port tolerances has been performed by UK within the worksharing project on spirotetramat). The proposed import tolerances are summarised in the following table.

Table B.7.13-1: Import tolerances

Commodity Proposed import tolerances according to the intended uses [mg/kg] 1) Comments

Citrus 1 Proposal by Canada: 0.6 mg/kg; difference between the two proposals based on different calculation-models and/or MRL-classes. Tree nuts 0.5 Proposal by Canada: 0.25 mg/kg; differ ence between the two proposals based on different calculation-models and/or MRL-classes. Almond hulls: 9 mg/kg (proposal Canada) is not considered as this is no food item in EU. Pome fruit 1 Proposal by UK 0.5 mg/kg (according to Me thod I and II calculation: 1 mg/kg might be more appropriate; covering Canada’s proposal of 0.7 mg/kg). Apricots 2 Extrapolation from NAFTA peach data Canada’s proposal: 4.5 mg/kg (group tolerance stone fruits – based on cherry data?) Cherries 5 Canada’s proposal: 4.5 mg/kg (group tole rance stone fruits) difference between the two proposalsbased on different calculation-models and/or MRLclasses. Peaches 2 Canada’s proposal: 4.5 mg/kg (group toler ance stone fruits – based on cherry data?) Plums 2 Based on 6 trials only (major crop in N-EU).. Proposal by Canada: 4.5 mg/kg; (group tolerance stone fruits – based on cherry data?)

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Commodity Proposed import tolerances according to the intended uses [mg/kg] 1) Comments

Grapes 2 Proposal by Canada: 1.3 mg/kg; difference between the two proposals based on different calculation-models and/or MRL-classes. Potatoes 0.5 Proposal doesn’t cover Canadas MRL of 0. 6 mg/kg: difference between the two proposals based on different calculation-models and/or MRL-classes. Peppers 2 Corresponding to MRL-proposal based on cri tical EU-GAP (glasshouse) Cucumbers 0.2 Corresponding to MRL-proposal based o n critical EU-GAP (glasshouse); Canada’s proposal: 0.3 mg/kg, based on different calculation models Cucurbits, inedible peel 0.3 Corresponds to proposa l by Canada Flowering brassica 2 Proposal by Canada: 2.5 mg/kg; difference between the two proposals based on different calculation-models and/or MRL-classes. Head cabbage 2 Proposal by Canada: 2.5 mg/kg; differ ence between the two proposals based on different calculation-models and/or MRL-classes. Leafy brassica 10 Proposal by Canada: 8.0 mg/kg; dif ference between the two proposals based on different calculation-models and/or MRL-classes. Lettuce (and other salad plants including Brassicacea ) --- Intended for use in NAFTA, but no residue trials submitted. Hops 20 Based on 3 trials only. Proposal by Canada: 1 0.0 mg/kg; difference between the two proposalsbased on different calculation-models and/or MRLclasses.



### B.7.14 Basis for differences, if any, in conclusion s reached having regard to established or

proposed CAC MRLs

No differences, as no CAC MRLs are established or p roposed at the moment.

B.7.15 Estimates of potential and actual dietary ex posure through diet and other means

(Annex IIA 6.9; Annex IIIA 8.10)

B.7.15.1 Estimation of the potential and actual exp osure through diet

B.7.15.2 Estimation of chronic exposure through die t

The long term risk assessment is based on the ADI ( 0.05 mg/kg bw/day). TMDI-calculation was carried ou t by means of the EFSA chronic acute RA model rev.2, including also the diet consumption data obtained from the European diet compiled in the WHO Publicat ion on Cultural and Global Diets, 1994; as well as the diet consumption data obtained from the new German diet (VELS intake model for a child of 16.15 kg bodyweight). The proposed MRLs / import tolerances were used for calculation.

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Table B.7.15.2-1: Theoretical Maximum Daily Intake (TMDI) of spirotetramat residues presented as % exhaustion of the Acceptable Daily Intake: Highest calculated TMDI values in % of ADI MS Diet Highest contributor to MS diet (in % of ADI) Commodity / group of commodities

58.4 DE child 24.1 Apples 47.8 NL child 12.7 Apples

46.5 WHO Cluster diet B 12.3 Tomatoes 33.4 IE adult 5.0 Wine grapes 29.3 FR toddler 5.2 Apples 27.5 PT General population 10.0 Wine grapes 25.9 FR all population 16.0 Wine grapes

25.0 WHO cluster diet D 4.1 Potatoes 24.6 WHO regional European diet 4.4 Tomatoes 24.4 SE general population 90th

percentile 4.2 Potatoes

24.4 WHO cluster diet E 6.4 Wine grapes 22.6 NL general 3.0 Oranges 22.4 ES child 4.3 Oranges

21.2 WHO Cluster diet F 3.4 Potatoes

20.7 ES adult 5.4 Lettuce 19.6 FR infant 5.0 Apples

19.0 IT kids/toddler 5.7 Tomatoes

18.4 IT adult 4.7 Tomatoes 18.2 UK Toddler 4.0 Oranges 18.1 PL general population 4.1 Apples 17.1 DK child 4.6 Apples 15.3 UK vegetarian 3.3 Wine grapes

15.0 UK Infant 3.3 Potatoes 13.8 DK adult 5.6 Wine grapes 13.3 UK Adult 4.3 Wine grapes 13.0 LT adult 3.7 Apples 10.1 FI adult 1.9 Oranges



### TMDI (range) in % of ADI: Minimum: 10 Maximum: 58

Conclusion : The estimated Theoretical Maximum Daily Intakes (TM DI) was below the ADI. A long-term intake of residu es of spirotetremat is unlikely to present a public he alth concern.

B.7.15.2.1 Estimation of acute exposure through die t

IESTI-calculation was carried out by means of the EFSA chronic acute RA model rev.2, including also the diet consumption data obtained from the new UK diet (Acute Intakes; 97.5th percentiles), as well as th e diet consumption data obtained from the new German diet (VELS intake model for a child of 16.15 kg bodyweight). The acute risk assessment is based on the ARfD (1 m g/kg bw). For each commodity the calculation is bas ed on the highest reported MS consumption per kg bw an d the corresponding unit weight from the MS with th e critical consumption. If no data on the unit weight was available from that MS an average European uni t weight was used for the IESTI calculation.

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In the IESTI 1 calculation, the variability factors were 10, 7 or 5 (according to JMPR manual 2002), f or lettuce a variability factor of 5 was used. In the IESTI 2 calculations, the variability factor s of 10 and 7 were replaced by 5. For lettuce the c alculation was performed with a variabilty factor of 3.

Table B.7.15.2.1-1: International Estimates Short T erm Intake (IESTI) of spirotetramat residues presented as % exhaustion of the Acute Reference Do se:

IESTI 1 IESTI 2 Highest % of ARfD Commodities Highest % of ARfD Com modities

67.6 Kale 48.3 Kale 37.1 Chinese cabbage 37.1 Chinese cabbage 13.5 Lettuce 13.2 Cauliflower 13.3 Oranges 13.1 Table grapes 13.2 Cauliflower 10.0 Kohlrabi 

### The results of the IESTI calculations are reported for at least 5 commodities. If the ARfD is exceeded for more than 5 commodities, all IESTI values > 90% of ARfD are reported.

Conclusion : No exceedance of the ARfD was identified. A short term intake of residues of spirotetremat is unlikely to present a public health risk

B.7.15.3 Estimation of the potential and actual exp osure through other means

No spirotetramat residues above 0.1 μg/L are expect ed to occur in drinking water. Spirotetramat residu e intake through drinking water can therefore be asse ssed as theoretical maximum: 0.2 μg spirotetramat/person/day assuming a daily consumpti on of 2 L water. This contribution is considered marginal compared to the theoretical maximal intake of spirotetramat through food of plant and animal origin.

B.7.16 Summary and evaluation of residue behaviour (Annex IIA 6.11.1; Annex IIIA 8.11)

The metabolism of [azaspirodecenyl-3- 14 

### C]-spirotetramat in plants was investigated in apples, lettuce, cotton and potatoes. Head lettuce was treated with two spray applications of [azaspi rodecenyl-3- 14 

### C]-spirotetramat, formulated as an oil-dispersion formula ( 100 OD ), at a total rate of 167 g a.i./ha (0.15 lbs a.i./ A). The two applications were made at a 14-day retreatment interval. Treated let tuce was harvested at maturity 7 days after the las t treatment. More than 95% of the total radioactive r esidue (TRR) in lettuce was extracted with acetonit rile (ACN)/water. The TRR was 3.13 mg-equiv./kg, calcula ted by summing extracts and post extraction solids. Over 91% of the extracted radioactivity was identif ied. Unchanged parent compound spirotetramat was t he major residue identified (55.9% TRR), followed by B YI 08330-enol (17.8%), BYI 08330-enol-glucoside (11.4% TRR), and BYI 08330-ketohydroxy (6.2% TRR). The metabolism of spirotetramat was investigated in potatoes (tuber & tops) following three spray applications of [azaspirodecenyl-3- 14 

### C]-spirotetramat, formulated as an oil dispersion ( 100 OD ), at a total rate of 308 g a.i./ha (0.275 lbs. a.i./A). The applicati ons were made at a 21-day re-treatment interval (RT I). Potato samples were harvested 14 days after the last treat ment. Approximately 80% of the total radioactive re sidue (TRR) in tuber, and 96% of the TRR in tops were ext racted with acetonitrile (ACN)/water. Enzymatic treatment of the extracted tuber released approxima tely 14% of the TRR. The TRR in tuber and tops was 0.255 mg-equiv./kg and 11.057 mg-equiv./kg, respect ively, calculated by summing extracts and post extraction solids. Parent spirotetramat was not ide ntified in potato tuber. The predominant metabolite identified was BYI 08330-enol (65.8% TRR), followed by BYI 08330-ketohydroxy (6.8% TRR) and BYI

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08330-desmethyl-enol (6.7% TRR) and several other m inor metabolites ( ≤ 2.5 % of the TRR). In potato tops, spirotetramat and BYI 08330-ketohydroxy were the ma jor residues identified. The metabolism of spirotetramat was investigated in apple (fruits & leaves) following two spray applications of [azaspirodecenyl-3- 14 

### C]-spirotetramat, formulated as an oil-dispersion f ormula ( 100 OD ), at a total rate of 1100 g a.i./ha (0.982 lb a.i./A). The first applica tion was at a growth stage 69 of the current BBCH c ode and the second application was 20 days later at growth stage 71, 2 months (63 days) before harvest. Total radioactive residue (TRR) amounted to 0.61 mg-equiv ./kg (apple) and 36.63 mg-equiv./kg (apple leaves). Approximately 49% in apple was surface residues was hed with dichloromethane. Washed apple extracted with acetonitrile (ACN)/water yielded 49.5% of the TRR leaving only 2.1% of the TRR as unextractable residues. Unchanged parent spirotetramat was the on ly residue detected in the surface wash. The predominant residue found in the extract was BYI 08 330-mono-hydroxy followed by BYI 08330-ketohydroxy, BYI 08330-di-hydroxy, BYI 08330-desmethyl-ketohydro xy, BYI 08330-enol, and the respective glycosides thereof. As in apple fruits, the major residue in a pple leaves was the unchanged spirotetramat (72% of the TRR). Other residues detected were BYI 08330-ketohy droxy, BYI 08330-enol, and glycoside isomers of BYI 08330-desmethyl-ketohydroxy. A BYI 08330-ketohydrox y-formiate-glycoside was also detected.

Major metabolic reaction involved the hydrolytic cleavage of the carbonate ester parent bond of the parent compound to form BYI 08330-enol. Further reduction of the double bond in the teramic acid moiety of BY I 08330-enol occurred to form the BYI 08330-mono-hydr oxy metabolite. Hydroxylation in the tetramic acid moiety resulted in BYI 08330-ketohydroxy. Demethyl ation of the methoxy group of the cyclohexyl ring resulted via a proposed intermediate (BYI 08330-des methyl-enol) in BYI 08330-desmethyl-ketohydroxy (af ter the corresponding hydroxylation). Oxidation of the methoxy group resulted in BYI 08330-ketohydroxyformiate. Partly, metabolites bearing a hydroxy gr oup were conjugated with glucose.

The metabolism of spirotetramat was investigated in cotton (gin trash, lint & undelinted seeds) following two spray applications of [azaspirodecenyl-3- 14 

### C]-spirotetramat, formulated as a suspension concen trate ( 240 SC ), at a total rate of 264 g a.i./ha/season (0.23 lb s. a.i./A). The first application was made at an ea rly growth stage (BBCH 15) at a rate of 91.7 g a.i./ha, and th e second at growth stage 85 (134 days interval) at a rate of 172.3 g a.i./ha. One immature cotton plant sample w as collected at 19 days after the first application . Cotton gin trash, lint and undelinted seed samples were ha rvested 39 days after the last treatment. The total radioactive residue (TRR) was 2.381 mg-equiv./kg in the immature plant sample, 1.641 mg-equiv./kg in g in trash, 1.078 mg-equiv./kg in lint, and 0.119 mg-equ iv./kg in undelinted seed. Parent compound, spirotetramat, was the major residue (46.95% TRR) i dentified in the immature cotton plant. Also found were 13 minor metabolites ranging from 0 .18% to 9.76% TRR. The major residues identified in cotton gin trash were BYI 08330-ketohydroxy (29.7% TRR), spirotetra mat (19.8% TRR), and BYI 08330-enol (12.1% TRR). The major residues identified in cott on lint were spirotetramat (32.3% TRR), BYI 08330- mandelic acid amide (11.9% TRR), and BYI 08330-keto hydroxy (10.5% TRR). The major residue found in the cotton undelinted seeds was BYI 08330-enol (39.8% TRR), while BYI 08330-ke tohydroxy represented 9.04% of the TRR (0.011 mg-equiv./kg). Ten metaboli tes representing 0.6-4.4% of the TRR (0.003-0.064 mg-equiv./kg) were also found in the gin trash, lin t and undelinted seeds. In cotton, cleavage of the pyrrolidine ring of BYI0 8330-ketohydroxy followed by decarboxylation and fu rther cleavage reactions led to the formation of BYI08330 -MA-amide, BYI08330-olefin, BYI08330-mandelic acid amide, and BYI08330-mandelic acid. Ring closure of the initial cleavage product formed BYI08330- hydroxymorpholinedione.

Livestock metabolism studies were performed in ruminants and poultry: Following 4 daily oral administrations of [azaspiro decenyl-3- 14 

### C]-spirotetramat to one lactating goat at a mean dose rate of 2.22 mg a.i./kg bw/day (73.03 mg/ kg in feed) given by gavage, concentrations of radioactivity in milk were low, reaching a maximum of 0.0261 mg equivalents/kg following the fourth do se. A plateau level in milk was reached within the run of the study (96 h). Approximately 90% of the adminis trated

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dose was eliminated via urine (78.4%), feces (11.6% ), milk (0.014%), and edible organs/tissues (0.061% ). The highest total radioactive residue (TRR) was obs erved in kidney (0.184 mg-equiv./kg) and liver (0.0 5 mgequiv./kg). Significantly lower residues were detec ted in the muscle and fat. The parent compound was not detected in samples of milk, muscle, fat, liver and kidney. The major metabolites detected were BYI 08330-enol (33.7-78.4 % of the TRR) and BYI 08330-enol-glucuronide (14.2- 37.4% of the TRR). Three other minor metabolites ( BYI 08330-ketohydroxy, BYI 08330-desmethyl-enol, an d BYI 08330-mono-hydroxy) were found each at less tha n 10% of the TRR. Following oral administration of [azaspirodecenyl-3

- 14 

### C]spirotetramat to 6 laying hens at a nominal dose level of 1.01 mg a.i./kg bw/day (12.86 mg/kg in feed) onc e daily for 14 consecutive days, concentrations of radioactivity in eggs reached a maximum of 0.014 -0 .016 mg equivalents/kg at day 6-14. The majority of the radioactivity (90% of the admin istered dose, AD) was detected in the excreta. Onl y 0.045% and 0.023% of the total AD were detected in the eggs and edible organs/tissues, respectively. The highest total radioactive residue (TRR) was detecte d in kidneys (0.039 mg-equiv./kg) and liver (0.017 mgequiv./kg), followed by fat (0.004 mg-equiv./kg), a nd muscle (0.003 mg-equiv./kg). The average TRR in eggs was 0.015 mg-equiv./kg. The parent compound was not detected in any of the samples. BYI 08330-enol was the major metabolite detected in eggs, liver, fat and muscle (18-84% of the TRR; 0.001-0.013 mg-equiv./kg). The glucuronic acid conjugate BYI 08330-enol-GA was also detected in eg gs (6.9% TRR), muscle (4.2% TRR) and liver (15.1% TRR). The biodegradation of spirotetramat in livestock can be characterized as cleavage of the carbonate ester group to the primary metabolite BYI 08330-enol foll owed by conjugation of the enol hydroxy group with glucuronic acid to BYI 08330-enol-GA. Oxidation of the azaspirodecenyl moiety to BYI 08330-ketohydrox y and demethylation of the methoxy group to BYI 08330 -desmethyl-enol were minor metabolic reactions in ruminants as well as reduction of the azaspirodecen yl moiety to BYI 08330-monohydroxy.

The residue definition for the expression of the MRL/monitoring and risk assessment for plant commodities are spirotetramat and the metabolites BYI 08330-en ol, BYI 08330-ketohydroxy, BYI08330- enol-Glc, and BYI 08330-mono-hydroxy. Based on the currently proposed uses, the residue d efinition for the expression of the MRL/monitoring for livestock commodities are spirotetramat and the metabolite BYI 08330-eno l and the residue definition for the risk assessment for livestock commodities are spirotetramat and th e metabolites BYI 08330-enol and BYI 08330-enol-GA. Relevant for EU: Considering that the residue definitions for enforc ement and for the riskassessment are different for food of animal origin, conversion factors could be proposed for the riskassessment based on the metabolism studies. Regarding the low-to-zero residue situatio n in food of animal origin shown in the livestock f eeding study, it is not considered necessary to propose co nversion factors.

Results from supervised residue trials in lettuce and citrus are reported representing th e designated intended uses of this Annex II dossier for Annex I inclusion of spirotetramat (BYI08330). In addition, residue data from uses of spirotetrama t in pome fruit, stone fruit, grapes, strawberries, onions, fruiting vegetables, brassica vegetables and hops a re reported and evaluated in order to accelerate th e fixing of MRLs with respect to Regulation 396/2005/EC. Thu s, all possible MRLs are “peer-reviewed” and there is no need for additional work load after Annex I – in clusion for spirotetramat (approach supported by EF SA).

Spirotetramat is applied as a spray solution to the different crops. Different formulations of spirote tramat were used: In 2004, residue trials were conducted w ith the OD 100 formulation of BYI08330. Due to a mi nor change of the final formulation from OD 100 to OD 1 50, residue trials in 2005 were conducted with the OD 150 formulation of BYI08330. The composition of bot h formulations is similar, but the amount of the ac tive substance is 100 g as/L in the OD 100 formulation a nd 150 g as/L in the OD 150 formulation. Applied at

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identical use rates for the active substance, both formulations are considered to be comparable with r espect to residues.

Results from additional residue trials are reported , which were conducted using a SC 240 formulation o r a SC 048 formulation of BYI08330 (with the addition o f 0.2 % rape methyl ester) to the spray solution. T he results of these trials are reported to give a comp lete picture of the BYI08330 residue behaviour.

Analysis of residue samples was conducted according to method 00875 (see Chapter IIA 4.3). The single analytes (spirotetramat and its metabolites BYI0833 0-enol, -ketohydroxy, -monohydroxy and -enol-glucos ide) are determined by HPLC-MS/MS. The results are expre ssed as parent equivalents. The total residue of spirotetramat is calculated by summing up the value s determined for the individual analytes expressed as parent equivalent. Expressed as parent equivalents the LOQ is 0.01 mg/kg for spirotetramat, 0.012 mg/k g for BYI08330-enol, -ketohydroxy and –monohydroxy and 0. 08 mg/kg for BYI08330-enol-glucoside. For hop cones the respective LOQs are by a factor of 10 hig her. The LOQ for the calculated total residue of BYI08330 is quoted at 0.054 mg/kg (hops 0.54 mg/kg)

.

Storage stability studies were conducted for all crops analysed for Spirotetramat residues. Adequate method-validation data were provided. Individual an alytes showed varying degrees of degradation over t he course of the study. Total residues (calculated as the summation of the single spiked analyte and all detectable analytes r esulting from the degradation of the spiked compound) were s table (<30% degradation) in tomato fruit, potato tu bers, lettuce heads, climbing French bean, and almond nut meat during frozen storage for up to 540 days. Total residues of spirotetramat in orange juice and prunes spiked with spirotetramat and the metabolit es BYI 08330-enol, BYI 08330-ketohydroxy, BYI 08330-mono-h ydroxy, BYI 08330-enol-Glc were stable (<30% degradation) during frozen storage for up to 144 da ys. The residues of wheat (hay, straw and grain), Swiss chard, and turnip (leaves and roots) from the conf ined rotational crop study stable after a storage period of at least 30 months.

For investigation of the effects on the nature of the residue during process ing , the behaviour of BYI 08330 and its four metabolites BYI08330-enol, BYI08 330-enol-glucoside, BYI08330-ketohydroxy and BYI08330-monohydroxy in buffer solution in three re presentative sets of hydrolysis conditions was stud ied. BYI 08330 was demonstrated to be resistant to hydro lysis under conditions being representative for pasteurization. Under conditions representative for baking, boiling and brewing 15 % of BYI 08330 degr aded to BYI08330-enol. Under conditions of sterilization the active substance was nearly completely hydroly sed to BYI08330-enol. BYI 08330-enol was detected as the o nly hydrolysis product. BYI 08330-enol was shown to be resistant to hydroly sis under all test conditions. BYI 08330-enol-glucoside was resistant to hydrolysi s under conditions representative for pasteurisatio n. Under conditions representative for baking, brewing and boiling ca.10 % of the test substance was hydrolysed to BYI 08330-enol. Under conditions of s terilization ca. 40 % of the BYI 08330-enol-glucosi de was hydrolysed to the enol metabolite. BYI 08330-ketohydroxy was demonstrated to be resist ant to hydrolysis under conditions of pasteurisatio n. Under conditions of baking, brewing and boiling a s light degradation to BYI 08330-MA-amide was found (5%). Under conditions of sterilisation BYI 08330-k etohydroxy was completely hydrolysed to BYI 08330-M Aamide. BYI 08330-monohydroxy was shown to be resistant und er all test conditions.

Relevant for EU: Estimation of the dietary burden for livestock anim als: Residues of Spirotetramat in animal feed might occu r after treatment of head and leafy brassica, when kale or/and cabbage are fed to livestock. Residues might also be found in animal feed after treatment of ci trus or

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pome fruit, when citrus dried pulp or apple wet pom ace are fed to cattle. The dietary burden, taking i nto account the highest residue, is 0.273 mg/kg diet fo r chicken and 1.91 mg/kg diet for dairy cattle. Although the dietary burden for chicken exceeds the trigger of 0.1 mg a.s./kg feed, no residues of tot al spirotetramat above 0.01 mg/kg are expected in edib le tissues or eggs with respect to the metabolism s tudy in laying hens. Therefore no feeding study in poult ry was required. In consequence of the dietary burden of 1.9 mg a.i. /kg feed (dry weight basis), a feeding study in dairy cattle was designed to quantify the residues found in tis sues and milk from dairy cows following oral administration of spirotetramat. Spirotetramat was administered via capsule to ten l actating Holstein dairy cows for 29 consecutive day s. The target dose rates (based on feed dry weight) were 0 mg/kg feed/day (control), 3.0 mg/kg feed/day, 9.0 mg/kg feed/day, or 30 mg/kg feed/day. Total spirotetramat residue in the milk samples fro m the 30-mg/kg feeding level were at or below the L OQ (0.005 mg/kg) in all cows throughout the study with the exception of a maximum residue of 0.006 mg/kg in one cow on study day 10. Residues of parent equival ents did not concentrate in samples of skim milk or milk fat separated from whole milk. A low tissue burden was observed, with the highest residues found in ki dney at the three dosing levels (0.022 mg/kg, 0.075 mg/k g and 0.274 mg/kg, respectively). At the 3-mg/kg do sing level, average residues of spirotetramat equivalent s were less than the LOQ (0.01 mg/kg) in fat, muscl e and liver.

Relevant for EU: Processing studies were conducted under household or industrial condi tions, respectively, to investigate the residue levels in the following fractions: Orange juice and marmalade; apple sauce and juice ( as well as possible feed item wet pomace); cherry f ruit preserve; raisins; wine; tomato juice, preserve and puree; cooked beans as well as beer. The resulting transfer factors (<1) show that no concentration of total spirotetramat residues takes place during pr ocessing, with the exception of apple wet pomace (transfer fa ctor 2.5) which is relevant for animal feed, and in raisins (transfer factor 2.7).

The metabolism in rotational crops (spring wheat, Swiss chard and turnips) was invest igated following spray application of [azaspirodecenyl-3-14C] spirot etramat onto bare soil at an application rate of 40 6 g a.i./ha. The total radioactive residues (TRRs) were highest in wheat straw of the 30-day rotation (0.9 98 mg/kg). In the 260-day rotation, only wheat hay and wheat straw showed residues above 0.01 mg/kg. A significant decline of TRRs from the 30-day to the 260-day rotation was observed in all raw agricultur al commodities (RACs). The lowest residues were genera lly detected in the edible matrices wheat grain and turnip roots, followed by Swiss chard. Parent compound spirotetramat was not detected in a ny sample. The percentage of conjugates increased from the 30-day to the 260-day rotation. The follow ing potential components of the residue definition (>10% TRR) were identified in the confined rotational cro p study: BYI08330, BYI08330-ketohydroxy, and free a nd conjugated BYI08330-desmethyl-ketohydroxy, BYI08330 -desmethyl-di-hydroxy and BYI-08330-ketohydroxyalcohol. None of these residues were found in the rotational crop field trials >0.020 mg/kg in/on all rotational crop matrices at a 30-day PBI.

Relevant for EU: The results of the confined rotational crop study u sing radiolabelled material show that residues resu lting from the use of spirotetramat in primary crops migh t lead to residues >LOQ in rotational crops, which are not covered by the residue definition for plant matrice s. The crop rotation field studies conducted in 3 d ifferent regions in the USA are considered acceptable as add itional information to elucidate, if the residue de finition for primary crops has to be enlarged or not. The expected residues in rotational crops are cover ed sufficiently by the residue definition for the e xpression of the MRL/monitoring and risk assessment for plant commodities (spirotetramat and the metabolites BYI

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08330-enol, BYI 08330-ketohydroxy, BYI08330-enol-Gl c, and BYI 08330-mono-hydroxy), based on the outcome of the field trials in succeeding crops, wh ich are accepted by RMS Austria as additional infor mation.

Table B.7.16-1: Key results of crop residue trials conducted with spirotetramat (with relevance to MRL-estimation; EU-uses)

Crop Application

[kg a.s./ha] Region 1) No. of trials PHI [days] Lowest

residue at harvest [mg/kg] 2) Highest residue at

harvest [mg/kg] 2)

Citrus 2 x 0.288 S 17 14 - 28 0.064 0.331 Lettuce 2 x 0.072 G 8 7 0.163 2.327

Pome fruit 2 x 0.216 N 13 21 - 27 0.064 0.254 Pome fruit 2 x 0.216 S 12 20 - 28 <0.054 0.249

Peach / Apricots 2 x 0.180 S 9 20 - 22 0.115 0.687

Plums 2 x 0.216 N 8 21 – 28 0.119 0.828 Plums 2 x 0.216 S 4 21 0.135 0.485 Cherries 2 x 0.216 N 7 21 – 28 0.248 0.939 Cherries 2 x 0.216 S 4 21 0.629 1.045 Grapes 2 x 0.096 S 10 14 – 15 0.167 0.641 Strawberries 2 x 0.096 G 8 3 – 7 0.205 0.328

Onions 4 x 0.072 N 8 7 – 8 <0.054 0.202 Onions 4 x 0.072 S 8 7 – 21 <0.054 0.172 Tomatoes 4 x 0.144 G 8 3 – 7 0.215 0.736 Peppers 4 x 0.1305 G 12 3 – 7 0.268 0.581 Cucumbers 4 x 0.144 G 8 3 <0.054 0.077 Melons 4 x 0.072 G 8 3 – 5 <0.054 0.057 Flowering brassica 3 x 0.072 N 9 3 – 14 0.11 0.578

Flowering brassica 3 x 0.072 S 4 3 – 14 0.130 0.439

Brussel sprouts 3 x 0.072 N 8 3 – 21 0.088 0.218

Head cabbage 3 x 0.072 N 10 3 – 14 0.067 0.261

Head cabbage 3 x 0.072 S 4 7 – 21 0.082 0.232

Leafy brassica 3 x 0.072 N 4 3 – 8 0.240 0.765

Leafy brassica 3 x 0.072 S 4 3 – 7 0.212 0.631

Kohlrabi 3 x 0.072 N 4 3 – 7 0.152 0.670 Green beans 4 x 0.144 G 8 14 – 21 0.082 0.624 Hops 2 x 0.175 N 8 13 - 22 1.11 4.34

1) N: Northern Region of Europe; S: Southern Region o f Europe 2) Residues expressed as spirotetramat



### Table B.7.16-2: MRL proposals for spirotetramat (ba sed on the intended uses / Import tolerances).

Commodity Proposed EU-MRLs according to the intended uses/import tolerances [mg/kg] 1) Comments

Citrus 1 Import tolerance (0.5 mg/kg based on EU-GAP) Lettuce 5 --- (No import tolerance. Intended for us e in NAFTA, but no residue data submitted.) Tree nuts 0.5 Import tolerance (no EU-GAP)

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Commodity Proposed EU-MRLs according to the intended uses/import tolerances [mg/kg] 1) Comments

Pome fruit 1 Import tolerance (0.3 mg/kg based on EU- GAP) Peach / Apricots 2 Import tolerance (1 mg/kg based on EU-GAP) Cherries 5 Import tolerance (1 mg/kg based on EU-GAP) Plums 2 Import tolerance (2 mg/kg also based on EU-GAP) Grapes 2 Import tolerance (1 mg/kg based on EU-GAP) Strawberries 1 --- Potatoes 0.5 Import tolerance (no EU-GAP) Onions 0.3 ---

Tomatoes 2 --- Peppers 2 Import tolerance (2 mg/kg also based on EU- GAP) Aubergines 2 Extrapolated from tomatoes. Cucumbers 0.2 Import tolerance (0.2 mg/kg also base d on EUGAP) Courgettes 0.2 Extrapolated from cucumbers. Cucurbits (inedible peel) 0.3 Import tolerance Flowering brassica 1 Import tolerance (1 mg/kg base d on EU-GAP) Brussel sprouts 0.3 --- Head cabbage 2 Import tolerance (0.5 mg/kg based on EU-GAP) Leafy brassica 10 Import tolerance (2 mg/kg based o n EU-GAP)

Kohlrabi 2 --- Green beans 2 --- Hops 20 Import tolerance (10 mg/kg based on EU-GAP) Kidney (bovine, goat, sheep, swine) 0.02 ---

1) Residues expressed in mg spirotetramat /kg

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B.7.17 References relied on

The grey marked studies are relevant for the EU-evaluation.

Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

Annex II Data and Information

KIIA 6.1.1 /01 Schoening, R.;

Wolters, A. 2006 Storage stability of BYI 08330 and its metabolites BYI08330-enol, BYI08330- ketohydroxy, BYI08330-mono-hydroxy and BYI08330-enol-glucoside in/on tomato (fruit), tomato (paste), potato (tuber), lettuce (head), climbing french bean ... Bayer CropScience AG, Report No.: MR-167/04, Edition Number: M-275244-01-2 Date: 27.07.2006 GLP, unpublished Yes BCS

KIIA 6.1.1 /02 Schoening, R.;

Wolters, A. 2006 Storage stability of BYI 08330 and its metabolites BYI08330-enol, BYI08330- ketohydroxy, BYI08330-mono-hydroxy and BYI08330-enol-glucoside in/on orange (juice) and prunes (fruit) for 5 months Bayer CropScience AG, Report No.: MR-06/076, Edition Number: M-276529-02-1 Date: 28.08.2006, Amended: 27.06.2007 GLP, unpublished Yes BCS

KIIA 6.1.1 /04 Schoening, R.;

Wolters, A. 2007 Storage stability of BYI 08330 and its metabolites BYI08330-enol, BYI08330- ketohydroxy, BYI08330-mono-hydroxy and BYI08330-enol-glucoside in/on tomato (fruit), tomato (paste), potato (tuber), lettuce (head), climbing French bean (bean with pod), and almond (nutmeat) for 24 months Bayer CropScience AG, Report No.: MR-07/268, Edition Number: M-289421-01-2 Date: 21.06.2007 GLP, unpublished Yes BCS

KIIA 6.2.1 /01 Haas, M.; Henk,

F. 2005 Metabolism of (azaspirodecenyl-3- 14C)BYI08330 in apple after spray application Bayer CropScience AG, Report No.: MEF-028/04, Edition Number: M-244827-01-3 Date: 25.01.2005 GLP, unpublished Yes BCS

KIIA 6.2.1 /02 Spiegel, K. 2006 Metabolism of [azaspirodecenyl-3-14C]BYI 08330 in cotton after spray application Bayer CropScience AG, Report No.: MEF-236/04, Edition Number: M-269105-01-2 Date: 03.03.2006 GLP, unpublished Yes BCS

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.2.1 /03 Haas, M.;

Diederich, B. 2004 Metabolism of [azaspirodecenyl-3- 14C]BYI08330 in lettuce Bayer CropScience AG, Report No.: MEF-049/04, Edition Number: M-242667-01-2 Date: 30.11.2004 GLP, unpublished Yes BCS

KIIA 6.2.1 /04 Sur, R. 2005 Metabolism of [azaspirodecenyl-3-14C]BYI 08330 in potatoes Bayer CropScience AG, Report No.: MEF-05/320, Edition Number: M-267707-01-2 Date: 05.12.2005 GLP, unpublished Yes BCS

KIIA 6.2.1 /05 Haas, M. 2004 Degradation of [azaspirodecenyl-3- 14C]BYI08330 by plant suspension cell cultures Bayer CropScience AG, Report No.: MEF-262/03, Edition Number: M-106579-01-2 Date: 21.01.2004 GLP, unpublished Yes BCS

KIIA 6.2.2 /01 Koester, J.;

Klempner, A. 2006 Metabolism of [azaspirodecenyl-3-14C]BYI 08330 in the laying hen Bayer CropScience AG, Report No.: MEF-05/273, Edition Number: M-268574-01-2 Date: 31.01.2006 GLP, unpublished Yes BCS

KIIA 6.2.3 /01 Koester, J.;

Klempner, A. 2006 [Azaspirodecenyl-3-14C]BYI 08330: Absorption, distribution, excretion, and metabolism in the lactating goat Bayer CropScience AG, Report No.: MEF-05/293, Edition Number: M-269256-01-2 Date: 16.03.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.1 /01 Schoening, R.;

Helfrich, P. 2005 Determination of the residues of BYI 08330 in/on orange after spraying of BYI 08330 (100 OD) in the field in Italy, Portugal and Spain Bayer CropScience AG, Report No.: RA-2032/04, Report includes Trial Nos.: 0139-04 0141-04 0239-04 0240-04 R 2004 0139/6 R 2004 0141/8 R 2004 0239/2 R 2004 0240/6 Edition Number: M-263546-01-1 Date: 21.12.2005 GLP, unpublished Yes BCS

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.1 /02 Schoening, R.;

Helfrich, P. 2006 Determination of the residues of BYI 08330 in/on mandarin after spraying of BYI 08330 (100 OD) in the field in Italy, Portugal and Spain Bayer CropScience AG, Report No.: RA-2033/04, Report includes Trial Nos.: 0142 - 04 0143 - 04 0237 - 04 0238 - 04 R 2004 0142/6 R 2004 0143/4 R 2004 0237/6 R 2004 0238/4 Edition Number: M-264450-01-1 Date: 19.01.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.1 /03 Schoening, R.;

Wieland, K. 2006 Determination of the residues of BYI 08330 in/on orange after spraying of BYI 08330 (150 OD) in the field in Portugal, Italy and Spain Bayer CropScience AG, Report No.: RA-2003/05, Report includes Trial Nos.: 0046-05 0047-05 0048-05 0049-05 R 2005 0046/7 R 2005 0047/5 R 2005 0048/3 R 2005 0049/1 Edition Number: M-269908-01-1 Date: 25.04.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.1 /04 Schoening, R.;

Wieland, K. 2006 Determination of the residues of BYI 08330 in/on mandarin after spraying of BYI 08330 (150 OD) in the field in Portugal, Spain and Italy Bayer CropScience AG, Report No.: RA-2002/05, Report includes Trial Nos.: 0041-05 0042-05 0043-05 0044-05 0045-05 R 2005 0041/6 R 2005 0042/4 R 2005 0043/2 R 2005 0044/0 R 2005 0045/9 Edition Number: M-270179-01-1 Date: 27.04.2006 GLP, unpublished Yes BCS

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.10 /01 Freitag, T.;

Helfrich, P. 2006 Determination of the residues of BYI 08330 in/on cherry tomato after spraying of BYI 08330 (100 OD) in the greenhouse in Italy and Spain Bayer CropScience AG, Report No.: RA-2139/04, Report includes Trial Nos.: 0823 - 04 0824 - 04 0825 - 04 0826 - 04 R 2004 0823/4 R 2004 0824/2 R 2004 0825/0 R 2004 0826/9 Edition Number: M-264462-01-1 Date: 17.01.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.10 /02 Freitag, T.;

Helfrich, P. 2005 Determination of the residues of BYI 08330 in/on tomato after spraying of BYI 08330 (100 OD) in the greenhouse in Greece, Spain and Italy Bayer CropScience AG, Report No.: RA-2140/04, Report includes Trial Nos.: 0827-04 0828-04 0829-04 0830-04 R 2004 0827/7 R 2004 0828/5 R 2004 0830/7 R 2004 0929/3 Edition Number: M-263523-01-1 Date: 20.12.2005 GLP, unpublished Yes BCS

KIIA 6.3.1.10 /03 Freitag, T.;

Helfrich, P. 2006 Determination of the residues of BYI 08330 in/on tomato after spraying of BYI 08330 (100 OD) in the field in Spain, Portugal, Greece and Italy Bayer CropScience AG, Report No.: RA-2130/04, Report includes Trial Nos.: 0849-04 0850-04 0852-04 0853-04 R 2004 0849/8 R 2004 0850/1 R 2004 0852/8 R 2004 0853/6 Edition Number: M-263566-01-1 Date: 10.01.2006 GLP, unpublished Yes BCS

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.11 /01 Schoening, R.;

Wolters, A. 2005 Determination of the residues of BYI 08330 in/on pepper after spraying of BYI 08330 (100 OD) in the greenhouse in the Netherlands, Germany, Southern France, Portugal, Italy and Spain Bayer CropScience AG, Report No.: RA-2026/04, Report includes Trial Nos.: 0113-04 0114-04 0115-04 0116-04 0117-04 0118-04 0119-04 0120-04 R 2004 0113/2 R 2004 0114/0 R 2004 0115/9 R 2004 0116/7 R 2004 0117/5 R 2004 0118/3 R 2004 0119/1 R 2004 0120/5 Edition Number: M-259820-01-1 Date: 02.11.2005 GLP, unpublished Yes BCS

KIIA 6.3.1.11 /02 Schoening, R.;

Wolters, A. 2005 Determination of the residues of BYI 08330 in/on pepper after spraying of BYI 08330 (100 OD) in the field in Spain, Southern France, Italy and Portugal Bayer CropScience AG, Report No.: RA-2027/04, Report includes Trial Nos.: 0121-04 0122-04 0124-04 0125-04 R 2004 0121/3 R 2004 0122/1 R 2004 0124/8 R 2004 0125/6 Edition Number: M-260011-01-1 Date: 07.11.2005 GLP, unpublished Yes BCS

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.11 /03 Schoening, R.;

Helfrich, P. 2006 Determination of the residues of BYI 08330 in/on pepper after spraying of BYI 08330 (240 SC) in the greenhouse in Southern France, Germany, Italy and Portugal Bayer CropScience AG, Report No.: RA-2134/04, Report includes Trial Nos.: 0791-04 0792-04 0793-04 0794-04 R 2004 0791/2 R 2004 0792/0 R 2004 0793/9 R 2004 0794/7 Edition Number: M-263426-01-1 Date: 09.01.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.11 /04 Schoening, R.;

Wolters, A. 2006 Determination of the residues of BYI 08330 in/on pepper after spraying of BYI 08330 (150 OD) in the field in Italy and Portugal Bayer CropScience AG, Report No.: RA-2039/05, Report includes Trial Nos.: 0200-05 0202-05 R 2005 0200/1 R 2005 0202/8 Edition Number: M-266615-01-1 Date: 21.02.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.11 /05 Schoening, R.;

Wolters, A. 2006 Determination of the residues of BYI 08330 in/on pepper after spraying of BYI 08330 (048 SC) in the field in Italy and Portugal Bayer CropScience AG, Report No.: RA-2046/05, Report includes Trial Nos.: 0707-05 0708-05 R 2005 0707/0 R 2005 0708/9 Edition Number: M-266682-01-1 Date: 21.02.2006 GLP, unpublished Yes BCS

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.12 /01 Cavaille, C. 2005 Determination of the residues of BYI 08330 in/on cucumber after spraying of BYI 08330 (100 OD) in the greenhouse in Germany, Italy, Spain and Greece Bayer CropScience, CRLD, Lyon, France Bayer CropScience AG, Report No.: RA-2030/04, Report includes Trial Nos.: 0130-04 0131-04 0132-04 0133-04 0134-04 0135-04 0136-04 0138-04 R20040130/2 R20040131/0 R20040132/9 R20040133/7 R20040134/5 R20040136/1 R20040138/8 Edition Number: M-259128-01-1 Date: 21.10.2005 GLP, unpublished Yes BCS

KIIA 6.3.1.12 /02 Cavaille, C. 2005 Determination of the residues of BYI 08330 in/on cucumber after spraying of BYI 08330 (100 OD) in the field in Spain and Italy Bayer CropScience AG, Report No.: RA-2028/04, Report includes Trial Nos.: 0126-04 0128-04 0129-04 R20040126/4 R20040128/0 R20040129/9 Edition Number: M-259667-01-1 Date: 02.11.2005 GLP, unpublished Yes BCS

KIIA 6.3.1.12 /03 Ballesteros, C. 2006 Determination of the residues of BYI 08330 in/on cucumber after spraying of BYI 08330 (150 OD) in the field in Spain and Italy Bayer CropScience SA, Centre de Recherche de La Dargoire, Lyon, France Bayer CropScience AG, Report No.: RA-2043/05, Report includes Trial Nos.: R 2005 0239/7 R 2005 0240/0 R 2005 0241/9 R 2005 0715/1 Edition Number: M-268869-01-1 Date: 03.04.2006 GLP, unpublished Yes BCS

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.13 /01 Cavaille, C. 2005 Determination of the residues of BYI 08330 in/on melon after spraying of BYI 08330 (100 OD) in the greenhouse in Italy, Spain, Southern France, and Portugal Bayer CropScience, Development - Residues, Operator and Concumer Safety, CRLD, Lyon, France Bayer CropScience AG, Report No.: RA-2128/04, Report includes Trial Nos.: 0836-04 0837-04 0838-04 0839-04 0840-04 0841-04 0881-04 0883-04 R20040836/6 R20040837/4 R20040838/2 R20040839/0 R20040840/4 R20040841/2 R20040881/1 R20040883/0 Edition Number: M-259446-01-1 Date: 27.10.2005 GLP, unpublished Yes BCS

KIIA 6.3.1.13 /02 Cavaille, C. 2005 Determination of the residues of BYI 08330 in/on melon after spraying of BYI 08330 (100 OD) in the field in Italy, Spain and Greece Bayer CropScience, Development - Residues, Operator and Consumer Safety, CRLD, Lyon, France Bayer CropScience AG, Report No.: RA-2129/04, Report includes Trial Nos.: 0842-04 0843-04 0844-04 0845-04 R20040842/0 R20040843/9 R20040844/7 R20040845/5 Edition Number: M-259449-01-1 Date: 27.10.2005 GLP, unpublished Yes BCS

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.13 /03 Ballesteros, C. 2006 Determination of the residues of BYI 08330 in/on melon after spraying of BYI 08330 (150 OD) in the field in Greece, Spain, Portugal and Italy Bayer CropScience SA, Lyon, France Bayer CropScience AG, Report No.: RA-2042/05, Report includes Trial Nos.: R 2005 0230/3 = 0230 - 05 R 2005 0231/1 = 0231 - 05 R 2005 0233/8 = 0233 - 05 R 2005 0234/6 = 0234 - 05 R 2005 0717/8 = 0717 - 05 Edition Number: M-268388-02-1 Date: 16.03.2006, Amended: 09.08.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.14 /01 Bardel, P.;

Freitag, T. 2005 Determination of the residues of BYI 08330 in/on broccoli after spraying of BYI 08330 (100 OD) in the field in Germany and United Kingdom Bayer CropScience AG, Report No.: RA-2022/04, Report includes Trial Nos.: 0105-04 0108-04 R 2004 0105/1 R 2004 0108/6 Edition Number: M-259571-01-1 Date: 25.10.2005 GLP, unpublished Yes BCS

KIIA 6.3.1.14 /02 Zimmer, D.;

Freitag, T. 2005 Determination of the residues of BYI 08330 in/on cauliflower after spraying of BYI 08330 (100 OD) in the field in Germany and France Bayer AG, Leverkusen, Germany Bayer CropScience AG, Report No.: RA-2023/04, Report includes Trial Nos.: 0109-04 0110-04 R 2004 0109/4 R 2004 0110/8 Edition Number: M-259580-01-1 Date: 26.10.2005 GLP, unpublished Yes BCS

KIIA 6.3.1.14 /03 Bardel, P.;

Freitag, T. 2005 Determination of the residues of BYI 08330 in/on broccoli after spraying of BYI 08330 (100 OD) in the field in Italy Bayer CropScience AG, Report No.: RA-2024/04, Report includes Trial Nos.: 0111-04 R 2004 0111/6 Edition Number: M-259272-01-1 Date: 21.10.2005 GLP, unpublished Yes BCS

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.14 /04 Zimmer, D.;

Freitag, T. 2005 Determination of the residues of BYI 08330 in/on cauliflower after spraying of BYI 08330 (100 OD) in the field in France Bayer CropScience AG, Report No.: RA-2025/04, Report includes Trial Nos.: 0112-04 R 2004 0112/4 Edition Number: M-258975-01-1 Date: 18.10.2005 GLP, unpublished Yes BCS

KIIA 6.3.1.14 /05 Freitag, T.;

Wieland, K. 2006 Determination of the residues of BYI 08330 in/on broccoli and cauliflower after spraying of BYI 08330 (150 OD) in the field in Germany, Northern France and United Kingdom Bayer CropScience AG, Report No.: RA-2062/05, Report includes Trial Nos.: 0363-05 0364-05 0365-05 1017-05 1047-05 R 2005 0363/6 R 2005 0364/4 R 2005 0365/2 R 2005 1017/9 R 2005 1047/0 Edition Number: M-275226-01-1 Date: 26.07.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.14 /06 Freitag, T.;

Wieland, K. 2006 Determination of the residues of BYI 08330 in/on broccoli and cauliflower after spraying of BYI 08330 (150 OD) in the field in Italy and Spain Bayer CropScience AG, Report No.: RA-2063/05, Report includes Trial Nos.: 0360-05 0362-05 R 2005 0360/1 R 2005 0362/8 Edition Number: M-275233-01-1 Date: 27.07.2006 GLP, unpublished Yes BCS

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.15 /01 Freitag, T.;

Wolters, A. 2005 Determination of the residues of BYI 08330 in/on brussels sprouts after spraying of BYI 08330 (100 OD) in the field in Germany and Northern France Bayer CropScience AG, Report No.: RA-2039/04, Report includes Trial Nos.: 0160-04 0161-04 0162-04 0163-04 R 2004 0160/4 R 2004 0161/2 R 2004 0162/0 R 2004 0163/9 Edition Number: M-260437-01-1 Date: 10.11.2005 GLP, unpublished Yes BCS

KIIA 6.3.1.15 /02 Freitag, T.;

Eberhardt, R.; Wolters, A. 2006 Determination of the residues of BYI 08330 in/on brussels sprouts after spraying of BYI 08330 (150 OD) in the field in Germany, Northern France and United Kingdom Bayer CropScience AG, Report No.: RA-2066/05, Report includes Trial Nos.: 0369 - 05 0370 - 05 0371 - 05 0372 - 05 R 2005 0369/5 R 2005 0370/9 R 2005 0371/7 R 2005 0372/5 Edition Number: M-273238-01-1 Date: 21.06.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.16 /01 Freitag, T.;

Wolters, A. 2005 Determination of the residues of BYI 08330 in/on round cabbage, red cabbage and savoy cabbage after spraying of BYI 08330 (100 OD) in the field in Germany, United Kingdom and Northern France Bayer CropScience AG, Report No.: RA-2037/04, Report includes Trial Nos.: 0152-04 0156-04 0157-04 R 2004 0152/3 R 2004 0156/6 R 2004 0157/4 Edition Number: M-260141-01-1 Date: 02.11.2005 GLP, unpublished Yes BCS

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.16 /02 Freitag, T.;

Behn, U. 2005 Determination of the residuesof BYI 08330 in/on red cabbage and round cabbage after spraying of BYI 08330 (100 OD) in the field in Spain and Italy Bayer AG, Leverkusen, Germany Bayer CropScience AG, Report No.: RA-2038/04, Report includes Trial Nos.: 0158-04 0159-04 R 2004 0158/2 R 2004 0159/0 Edition Number: M-260014-01-1 Date: 07.11.2005 GLP, unpublished Yes BCS

KIIA 6.3.1.16 /03 Ballesteros,

Gateaud, L. 2006 Determination of the residues of BYI 08330 in/on red cabbage, round cabbage and Savoy cabbage after spraying of BYI 08330 (150 OD) in the field in Northern-France and Germany Bayer CropScience SA, Lyon, France Bayer CropScience AG, Report No.: RA-2060/05, Report includes Trial Nos.: R20050352/0=0352-05 R20050353/9=0353-05 R20050354/7=0354-05 R20050355/5=0355-05 R20050356/3=0356-05 R20050357/1=0357-05 R20050359/8=0359-05 Edition Number: M-272557-01-1 Date: 09.06.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.16 /04 Ballesteros,

Gateaud, L. 2006 Determination of the residues of BYI 08330 in/on red cabbage and round cabbage after spraying of BYI 08330 (150 OD) in the field in Italy and Spain Bayer CropScience SA, Lyon, France Bayer CropScience AG, Report No.: RA-2061/05, Report includes Trial Nos.: R20050350/4=0350-05 R20050351/2=0351-05 Edition Number: M-272570-01-1 Date: 12.06.2006 GLP, unpublished Yes BCS

### - 224 -

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.17 /01 Freitag, T.;

Eberhardt, R. 2006 Determination of the residues of BYI 08330 in/on curly kale after spraying of BYI 08330 (100 OD) in the field in United Kingdom and Germany Bayer CropScience AG, Report No.: RA-2040/04, Report includes Trial Nos.: 0164-04 0165-04 R 2004 0164/7 R 2004 0165/5 Edition Number: M-263745-01-1 Date: 11.01.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.17 /02 Cavaille, C. 2006 Amendment no. 1 - Determination of the residues of BYI 08330 in/on curly kale after spraying of BYI 08330 (150 OD) in the field in Germany Bayer CropScience SA, Lyon, France Bayer CropScience AG, Report No.: RA-2064/05, Report includes Trial Nos.: R20050367/9=0367-05 R20050368/7=0368-05 Edition Number: M-272573-02-1 Date: 12.06.2006, Amended: 20.07.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.17 /03 Freitag, T.;

Eberhardt, R. 2006 Determination of the residues of BYI 08330 in/on chinese kale after spraying of BYI 08330 (100 OD) in the field in southern France and Spain Bayer CropScience AG, Report No.: RA-2041/04, Report includes Trial Nos.: 0166 - 04 0167 - 04 R 2004 0166/3 R 2004 0167/1 Edition Number: M-264301-01-1 Date: 17.01.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.17 /04 Ballesteros, C.;

Gateaud, L. 2006 Determination of the residues of BYI 08330 in/on Chinese cabbage after spraying of BYI 08330 (150 OD) in the field in Spain and Italy Bayer CropScience SA, Lyon, France Bayer CropScience AG, Report No.: RA-2136/05, Report includes Trial Nos.: 0709-05 0710-05 R 2005 0709/7 R 2005 0710/0 Edition Number: M-273243-01-1 Date: 23.06.2006 GLP, unpublished Yes BCS

### - 225 -

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.18 /01 Freitag, T.;

Eberhardt, R. 2006 Determination of the residues of BYI 08330 in/on kohlrabi after spraying of BYI 08330 (100 OD) in the field in Germany and the Netherlands Bayer CropScience AG, Report No.: RA-2043/04, Report includes Trial Nos.: 0169-04 0170-04 R 2004 0169/8 R 2004 0170/1 Edition Number: M-265036-01-1 Date: 30.01.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.18 /02 Freitag, T.;

Eberhardt R. 2006 Determination of the residues of BYI 08330 in/on kohlrabi after spraying of BYI 08330 (150 OD) in the field in Germany Bayer CropScience AG, Report No.: RA-2065/05, Report includes Trial Nos.: 0373 - 05 0374 - 05 R 2005 0373/3 R 2005 0374/1 Edition Number: M-272128-01-1 Date: 31.05.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.19 /01 Schoening, R.;

Wolters, A. 2006 Determination of the residues of BYI 08330 in/on climbing french bean after spraying of BYI 08330 (100 OD) in the greenhouse in Italy, Germany and Southern France Bayer CropScience AG, Report No.: RA-2042/04, Report includes Trial Nos.: 0172-04 0173-04 0174-04 0175-04 0176-04 0177-04 0178-04 0179-04 R 2004 0172/8 R 2004 0173/6 R 2004 0174/4 R 2004 0175/2 R 2004 0176/0 R 2004 0177/9 R 2004 0178/7 R 2004 0179/5 Edition Number: M-263646-01-1 Date: 11.01.2006 GLP, unpublished Yes BCS

### - 226 -

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.2 /01 Schoening, R.;

Wolters, A. 2005 Determination of the residues of BYI 08330 in/on lettuce after spraying of BYI 08330 (100 OD) in the greenhouse in Germany, Southern France, Italy and Spain Bayer CropScience AG, Report No.: RA-2054/04, Report includes Trial Nos.: 0393-04 0394-04 0396-04 0397-04 0398-04 0399-04 0401-04 0402-04 R 2004 0393/3 R 2004 0394/1 R 2004 0396/8 R 2004 0397/6 R 2004 0398/4 R 2004 0399/2 R 2004 0401/8 R 2004 0402/6 Edition Number: M-262616-01-1 Date: 15.12.2005 GLP, unpublished Yes BCS

KIIA 6.3.1.2 /02 Schoening, R. 2006 Determination of the residues of BYI 08330 in/on lettuce after spraying of BYI 08330 (150 OD) in the greenhouse in Greece, France, Netherlands, Portugal, Germany and Spain Bayer CropScience AG, Report No.: RA-2170/05, Report includes Trial Nos.: 1023 - 05 1024 - 05 1026 - 05 1027 - 05 1028 - 05 1029 - 05 1030 - 05 1031 - 05 R 2005 1023/3 R 2005 1024/1 R 2005 1026/8 R 2005 1027/6 R 2005 1028/4 R 2005 1029/2 R 2005 1030/6 R 2005 1031/4 Edition Number: M-272108-01-1 Date: 31.05.2006 GLP, unpublished Yes BCS

### - 227 -

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.2 /03 Schoening, R.;

Behn, U. 2005 Determination of the residues of BYI 08330 in/on lettuce after spraying of BYI 08330 (240 SC) in the greenhosue in Germany, Italy and Spain Bayer CropScience AG, Report No.: RA-2113/04, Report includes Trial Nos.: 0685-04 0687-04 0688-04 0689-04 R 2004 0685/1 R 2004 0687/8 R 2004 0688/6 R 2004 0689/4 Edition Number: M-261625-01-1 Date: 15.11.2005 GLP, unpublished Yes BCS

KIIA 6.3.1.2 /04 Schoening, R.;

Wolters, A. 2005 Determination of the Residues of BYI 08330 in/on Lettuce after Spraying of BYI 08330 (100 OD) in the Field in the Netherlands and Germany Bayer CropScience AG, Report No.: RA-2052/04, Report includes Trial Nos.: 0385-04 0386-04 0387-04 0388-04 R 2004 0385/2 R 2004 0386/0 R 2004 0387/9 R 2004 0388/7 Edition Number: M-260209-01-1 Date: 03.11.2005 GLP, unpublished Yes BCS

KIIA 6.3.1.2 /05 Schoening, R.;

Behn, U. 2005 Determination of the residues of BYI 08330 in/on lettuce after spraying of BYI 08330 (100 OD) in the field in Southern France, Spain, Portugal and Italy Bayer CropScience AG, Report No.: RA-2053/04, Report includes Trial Nos.: 0389-04 0390-04 0391-04 0392-04 R 2004 0389/5 R 2004 0390/9 R 2004 0391/7 R 2004 0392/5 Edition Number: M-260382-01-1 Date: 08.11.2005 GLP, unpublished Yes BCS

### - 228 -

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.20 /01 Schoening, R.;

Wolters, A. 2005 Determination of the residues of BYI 08330 in/on potato after spraying of BYI 08330 (100 OD) in the field in Germany, Northern France and United Kingdom Bayer CropScience AG, Report No.: RA-2114/04, Report includes Trial Nos.: 0690-04 0691-04 0692-04 0693-04 R 2004 0690/8 R 2004 0691/6 R 2004 0692/4 R 2004 0693/2 Edition Number: M-259808-01-1 Date: 03.11.2005 GLP, unpublished Yes BCS

KIIA 6.3.1.20 /02 Schoening, R.;

Wolters, A. 2005 Determination of the residues of BYI 08330 in/on potato after spraying of BYI 08330 (100 OD) in the field in Southern France, Italy, Spain and Portugal Bayer AG, Leverkusen, Germany Bayer CropScience AG, Report No.: RA-2115/04, Report includes Trial Nos.: 0694-04 0695-04 0696-04 0697-04 R 2004 0694/0 R 2004 0695/9 R 2004 0696/7 R 2004 0697/5 Edition Number: M-262622-01-1 Date: 15.12.2005 GLP, unpublished Yes BCS

KIIA 6.3.1.21 /01 Schoening, R.;

Helfrich, P. 2006 Determination of the residues of BYI 08330 in/on hop after spraying of BYI 08330 (100 OD) in the field in Northern France and Germany Bayer CropScience AG, Report No.: RA-2036/04, Report includes Trial Nos.: 0148-04 0149-04 0150-04 0151-04 R 2004 0148/5 R 2004 0149/3 R 2004 0150/7 R 2004 0151/5 Edition Number: M-265047-01-1 Date: 27.01.2006 GLP, unpublished Yes BCS

### - 229 -

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.21 /02 Schoening, R. 2006 Determination of the residues of BYI 08330 in/on hop after spraying of BYI 08330 (150 OD) in the field in Germany and Northern France Bayer CropScience AG, Report No.: RA-2108/05, Report includes Trial Nos.: 0550 - 05 0551 - 05 0552 - 05 0553 - 05 R 2005 0550/7 R 2005 0551/5 R 2005 0552/3 R 2005 0553/1 Edition Number: M-272100-01-1 Date: 19.05.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.3 /01 Schoening, R.;

Eberhardt, R. 2006 Determination of the residues of BYI 08330 in/on apple and pear after spraying of BYI 08330 (150 OD) in the field in United Kingdom and Germany Bayer CropScience AG, Report No.: RA-2012/05, Report includes Trial Nos.: 0083-05 0085-05 0086-05 0087-05 1018-05 R 2005 0083/1 R 2005 0085/8 R 2005 0086/6 R 2005 0087/4 R 2005 1018/7 Edition Number: M-269314-01-1 Date: 06.04.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.3 /02 Schoening, R.;

Helfrich, P. 2006 Determination of the residues of BYI 08330 in/on apple and pear after spraying and low-volume spraying of BYI 08330 (240 SC) in the field in Germany, United Kingdom and Northern France Bayer CropScience AG, Report No.: RA-2138/04, Report includes Trial Nos.: 0809 - 04 0810 - 04 0811 - 04 0812 - 04 R 2004 0809/9 R 2004 0810/2 R 2004 0811/0 R 2004 0812/9 Edition Number: M-264454-01-1 Date: 18.01.2006 GLP, unpublished Yes BCS

### - 230 -

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.3 /03 Schoening, R.;

Helfrich, P. 2006 Determination of the residues of BYI 08330 in/on apple and pear after spraying and low-volume spraying of BYI 08330 (100 OD) in the field in Italy, Spain and Southern France Bayer CropScience AG, Report No.: RA-2137/04, Report includes Trial Nos.: 0805 - 04 0806 - 04 0807 - 04 0808 - 04 R 2004 0805/6 R 2004 0806/4 R 2004 0807/2 R 2004 0808/0 Edition Number: M-264357-01-1 Date: 18.01.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.3 /04 Schoening, R.;

Eberhardt, R. 2006 Determination of the residues of BYI 08330 in/on apple and pear after spraying of BYI 08330 (150 OD) in the field in Southern France and Italy Bayer CropScience AG, Report No.: RA-2015/05, Report includes Trial Nos.: 0088-05 0089-05 0090-05 0091-05 R 2005 0088/2 R 2005 0089/0 R 2005 0090/4 R 2005 0091/2 Edition Number: M-268258-01-1 Date: 16.03.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.3 /05 Schoening, R.;

Helfrich, P. 2006 Determination of the residues of BYI 08330 in/on apple and pear after spraying and low-volume spraying of BYI 08330 (240 SC) in the field in Italy, Spain and Southern France Bayer CropScience AG, Report No.: RA-2136/04, Report includes Trial Nos.: 0800 - 04 0801 - 04 0802 - 04 0804 - 04 R 2004 0800 /5 R 2004 0801/3 R 2004 0802/1 R 2004 0804/8 Edition Number: M-264397-01-1 Date: 19.01.2006 GLP, unpublished Yes BCS

### - 231 -

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.3 /06 Schoening, R.;

Helfrich, P. 2005 Determination of the residues of BYI 08330 in/on apple and pear after spraying and low-volume spraying of BYI 08330 (100 OD) in the field in Germany, United Kingdom and Northern France Bayer CropScience AG, Report No.: RA-2135/04, Report includes Trial Nos.: 0795-04 0796-04 0797-04 0799-04 R 2004 0795/5 R 2004 0796/3 R 2004 0797/1 R 2004 0799/8 Edition Number: M-262625-02-2 Date: 15.12.2005, Amended: 29.05.2007 GLP, unpublished Yes BCS

KIIA 6.3.1.4 /01 Schoening, R.;

Wolters, A. 2005 Determination of the residues of BYI 08330 in/on peach and apricot after spraying of BYI 08330 (100 OD) in the field in Northern France and Germany Bayer CropScience AG, Report No.: RA-2126/04, Report includes Trial Nos.: 0785-04 0786-04 R 2004 0785/8 R 2004 0786/6 Edition Number: M-259798-01-1 Date: 02.11.2005 GLP, unpublished Yes BCS

KIIA 6.3.1.4 /02 Schoening, R.;

Eberhardt, R. 2006 Determination of the residues of BYI 08330 in/on apricot and peach after spraying of BYI 08330 (150 OD) in the field in Germany and Northern France Bayer CropScience AG, Report No.: RA-2006/05, Report includes Trial Nos.: 0059-05 0060-05 0061-05 R 2005 0059/9 R 2005 0060/2 R 2005 0061/0 Edition Number: M-268003-01-1 Date: 14.03.2006 GLP, unpublished Yes BCS

### - 232 -

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.4 /03 Schoening, R.;

Helfrich, P. 2006 Determination of the residues of BYI 08330 in/on peach and apricot after spraying of BYI 08330 (100 OD) in the field in Spain and Italy Bayer CropScience AG, Report No.: RA-2127/04, Report includes Trial Nos.: 0787-04 0788-04 0789-04 0790-04 R 2004 0787/4 R 2004 0788/2 R 2004 0789/0 R 2004 0790/4 Edition Number: M-263878-01-1 Date: 11.01.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.4 /04 Schoening, R.;

Eberhardt, R. 2006 Determination of the residues of BYI 08330 in/on apricot and peach after spraying of BYI 08330 (150 OD) in the field in Portugal, Spain, Greece, Southern France and Italy Bayer CropScience AG, Report No.: RA-2007/05, Report includes Trial Nos.: 0062-05 0063-05 0064-05 0065-05 0066-05 R 2005 0062/9 R 2005 0063/7 R 2005 0064/5 R 2005 0065/3 R 2005 0066/1 Edition Number: M-268094-01-1 Date: 14.03.2006 GLP, unpublished Yes B BCS

KIIA 6.3.1.5 /01 Schoening, R.;

Helfrich, P. 2006 Determination of the residues of BYI 08330 in/on plum after spraying of BYI 08330 (100 OD) in the field in Germany, Northern France and United Kingdom Bayer CropScience AG, Report No.: RA-2124/04, Report includes Trial Nos.: 0774-04 0775-04 0776-04 0777-04 R 2004 0774/2 R 2004 0775/0 R 2004 0776/9 R 2004 0777/7 Edition Number: M-263688-01-1 Date: 10.01.2006 GLP, unpublished Yes Bayer CropScience

### - 233 -

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.5 /02 Schoening, R. 2006 Determination of the residues of BYI 08330 in/on plum after spraying of BYI 08330 (150 OD) in the field in United Kingdom, Northern France and Germany Bayer CropScience AG, Report No.: RA-2004/05, Report includes Trial Nos.: 0050-05 0051-05 0052-05 0054-05 R 2005 0050/5 R 2005 0051/3 R 2005 0052/1 R 2005 0054/8 Edition Number: M-266052-01-1 Date: 09.02.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.5 /03 Schoening, R.;

Wolters, A. 2005 Determination of the residues of BYI 08330 in/on plum after low-volume spraying and spraying of BYI 08330 (100 OD) in the field in Southern France and Italy Bayer CropScience AG, Report No.: RA-2125/04, Report includes Trial Nos.: 0778-04 0779-04 R 2004 0778/5 R 2004 0779/3 Edition Number: M-262626-01-1 Date: 15.12.2005 GLP, unpublished Yes BCS

KIIA 6.3.1.5 /04 Schoening, R. 2006 Determination of the residues of BYI 08330 in/on plum after spraying of BYI 08330 (150 OD) in the field in Italy and Spain Bayer CropScience AG, Report No.: RA-2005/05, Report includes Trial Nos.: 0055-05 0058-05 R 2005 0055/6 R 2005 0058/0 Edition Number: M-266062-01-1 Date: 07.02.2006 GLP, unpublished Yes BCS

### - 234 -

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.6 /01 Schoening, R.;

Behn, U.; Wolters, A. 2006 Determination of the residues of BYI 08330 in/on sweet cherry and sour cherry after spraying of BYI 08330 (100 OD) in the field in Northern France and Germany Bayer CropScience AG, Report No.: RA-2119/04, Report includes Trial Nos.: 0718-04 0720-04 0721-04 0723-04 R 2004 0718/1 R 2004 0720/3 R 2004 0721/1 R 2004 0723/8 Edition Number: M-263879-01-1 Date: 12.01.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.6 /02 Schoening, R.;

Raecker, T. 2006 Determination of the residues of BYI 08330 in/on sweet cherry and sour cherry after spraying of BYI 08330 (150 OD) in the field in Germany and Northern France Bayer CropScience AG, Report No.: RA-2008/05, Report includes Trial Nos.: 0068-05 0071-05 0072-05 R 2005 0068/8 R 2005 0071/8 R 2005 0072/6 Edition Number: M-267524-01-1 Date: 06.03.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.6 /03 Schoening, R.;

Wolters, A. 2005 Determination of the resideus of BYI 08330 in/on sweet cherry after spraying of BYI 08330 (100 OD) in the field in Italy and Southern France Bayer CropScience AG, Report No.: RA-2118/04, Report includes Trial Nos.: 0716-04 0717-04 R 2004 0716/5 R 2004 0717/3 Edition Number: M-260405-01-1 Date: 08.11.2005 GLP, unpublished Yes BCS

### - 235 -

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.6 /04 Schoening, R.;

Eberhardt, R. 2006 Determination of the residues of BYI 08330 in/on sweet cherry after spraying of BYI 08330 (150 OD) in the field in Italy and Spain Bayer CropScience AG, Report No.: RA-2009/05, Report includes Trial Nos.: 0073-05 0074-05 R 2005 0073/4 R 2005 0074/2 Edition Number: M-267488-01-1 Date: 06.03.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.7 /01 Schoening, R.;

Eberhardt, R. 2006 Determination of the residues of BYI 08330 in/on grape and table grape after spraying and low-volume spraying of BYI 08330 (100 OD) in the field in Italy, Greece, Spain and Southern France Bayer CropScience AG, Report No.: RA-2049/04, Report includes Trial Nos.: 0196-04 0197-04 0198-04 0201-04 0202-04 0203-04 R 2004 0196/5 R 2004 0197/3 R 2004 0198/1 R 2004 0201/5 R 2004 0202/3 R 2004 0203/1 Edition Number: M-263864-01-1 Date: 12.01.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.7 /02 Ballesteros, C.;

Gateaud, L. 2006 Determination of the residues of BYI 08330 in/on grape after spraying of BYI 08330 (150 OD) in the field in Spain and Italy Bayer CropScience SA, Lyon, France Bayer CropScience AG, Report No.: RA-2034/05, Report includes Trial Nos.: R20050157/9=0157-05 R20050158/7=0158-05 Edition Number: M-270088-01-1 Date: 02.05.2006 GLP, unpublished Yes BCS

### - 236 -

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.7 /03 Ballesteros, C.;

Gateaud, L. 2006 Determination of the residues of BYI 08330 in/on grape after low-volume spraying and spraying of BYI 08330 (048 SC) in the field in Southern-France and Italy Bayer CropScience SA, Lyon, France Bayer CropScience AG, Report No.: RA-2036/05, Report includes Trial Nos.: 0161-05 0162-05 R20050161/7 R20050162/5 Edition Number: M-273708-01-1 Date: 24.04.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.8 /01 Freitag, T.;

Eberhardt, R. 2006 Determination of the residues of BYI 08330 in/on strawberry after spraying of BYI 08330 (100 OD) in the greenhouse in Germany and France Bayer CropScience AG, Report No.: RA-2122/04, Report includes Trial Nos.: 0726-04 0765-04 0766-04 0768-04 0769-04 0771-04 0772-04 0773-04 R 2004 0726/2 R 2004 0765/3 R 2004 0766/1 R 2004 0768/8 R 2004 0769/6 R 2004 0771/8 R 2004 0772/6 R 2004 0773/4 Edition Number: M-263736-01-1 Date: 11.01.2006 GLP, unpublished Yes BCS

### - 237 -

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.8 /02 Freitag, T.;

Helfrich, P. 2005 Determination of the residues of BYI 08330 in/on strawberry after spraying of BYI 08330 (100 OD) in the field in Germany and Northern France Bayer CropScience AG, Report No.: RA-2120/04, Report includes Trial Nos.: 0724-04 0759-04 0760-04 0761-04 R 2004 0724/6 R 2004 0759/9 R 2004 0760/2 R 2004 0761/0 Edition Number: M-262423-02-1 Date: 14.12.2005, Amended: 18.01.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.8 /03 Freitag, T.;

Helfrich, P. 2005 Determination of the residues of BYI 08330 in/on strawberry after spraying of BYI 08330 (100 OD) in the field in Italy, Spain and Southern France Bayer CropScience AG, Report No.: RA-2121/04, Report includes Trial Nos.: 0725-04 0762-04 0763-04 0764-04 R 2004 0725/4 R 2004 0762/9 R 2004 0763/7 R 2004 0764/5 Edition Number: M-262418-02-1 Date: 14.12.2005, Amended: 18.01.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.9 /01 Cavaille, C. 2005 Determination of the residues of BYI 08330 in/on onion after spraying of BYI 08330 (100 OD) in the field in Germany and Northern France Bayer CropScience S.A., Lyon, France Bayer CropScience AG, Report No.: RA-2131/04, Report includes Trial Nos.: 0854-04 0855-04 0856-04 0857-04 R20040854/4 R20040855/2 R20040856/0 R20040857/9 Edition Number: M-259115-01-1 Date: 21.10.2005 GLP, unpublished Yes BCS

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.1.9 /02 Ballesteros, C.;

Gateaud, L. 2006 Determination of the residues of BYI 08330 in/on onion after spraying of BYI 08330 (150 OD) in the field in United Kingdom, Northern-France and Germany Bayer CropScience SA, Centre de Recherche de La Dargoire, Lyon, France Bayer CropScience AG, Report No.: RA-2040/05, Report includes Trial Nos.: R 2005 0212/5 R 2005 0214/1 R 2005 0216/8 R 2005 0217/6 Edition Number: M-269474-01-1 Date: 14.04.2006 GLP, unpublished Yes BCS

KIIA 6.3.1.9 /03 Cavaille, C. 2005 Determination of the residues of BYI 08330 in/on onion after spraying of BYI 08330 (100 OD) in the field in Southern France, Greece, Italy and Spain Bayer CropScience, Lyon, France Bayer CropScience AG, Report No.: RA-2132/04, Report includes Trial Nos.: 0858-04 0859-04 0860-04 0861-04 R20040858/7 R20040859/5 R20040860/9 R20040861/7 Edition Number: M-259663-01-1 Date: 02.11.2005 GLP, unpublished Yes BCS

KIIA 6.3.1.9 /04 Ballesteros, C.;

Gateaud, L. 2006 Determination of the residues of BYI 08330 in/on onion after spraying of BYI 08330 (150 OD) in the field in Italy, Spain and Southern-France Bayer CropScience SA, Lyon, France Bayer CropScience AG, Report No.: RA-2041/05, Report includes Trial Nos.: R20050225/7=0225-05 R20050226/5=0226-05 R20050227/3=0227-05 R20050228/1=0228-05 Edition Number: M-269869-01-1 Date: 24.04.2006 GLP, unpublished Yes BCS

### - 239 -

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.2.1 /01 Freeseman, P.

L. 2006 BYI08330 150 OD and BYI08330 240 SC - Magnitude of the residue in/on brassica leafy vegetables (crop subgroup 5A, head and stern brassica, and 5B, leafy brassica greens) including residue reduction information Bayer CropScience, Stilwell, KS, USA Bayer CropScience AG, Report No.: RAFNY003, Edition Number: M-277100-01-1 Date: 31.08.2006 GLP, unpublished Yes BCS

KIIA 6.3.2.10 /01 Mackie, S. J.

W.; Harbin, A. M. 2006 BYI08330 150 OD and BYI08330 240 SC - Magnitude of the residue on stone fruit (crop group 12 - including residue reduction samples) Bayer CropScience, Stilwell, KS, USA Bayer CropScience AG, Report No.: RAFNY001, Edition Number: M-277063-01-1 Date: 31.08.2006 GLP, unpublished Yes BCS

KIIA 6.3.2.11 /01 Rupprecht, J. K. 2006 BYI08330 150 OD and BYI08330 240 SC - Magnitude of the residue on tree nuts (crop group 14) Bayer CropScience, Stilwell, KS, USA Bayer CropScience AG, Report No.: RAFNY010, Edition Number: M-277323-01-1 Date: 01.09.2006 GLP, unpublished Yes BCS

KIIA 6.3.2.2 /01 Duah, F. K. 2006 BYI08330 150 OD and BYI08330 240 SC - Magnitude of the residue in/on curcubit vegetables (crop group 9, including residue reduction information) Bayer CropScience, Stilwell, KS, USA Bayer CropScience AG, Report No.: RAFNY007, Edition Number: M-277110-01-1 Date: 31.08.2006 GLP, unpublished Yes BCS

KIIA 6.3.2.3 /01 Mackie, S. J. W. 2006 BYI08330 150 OD and BYI08330 240 SC - Magnitude of the residue on fruiting vegetables (crop group 8 - tomato, bell pepper, non-bell pepper) (including residue reduction information) Bayer CropScience, Stilwell, KS, USA Bayer CropScience AG, Report No.: RAFNY006, Edition Number: M-277197-01-1 Date: 31.08.2006 GLP, unpublished Yes BCS

### - 240 -

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.3.2.4 /01 Fischer, D. R. 2006 BYI08330 150 OD and BYI08330 240 SC - Magnitude of the residue in/on leafy vegetables Bayer CropScience, Stilwell, KS, USA Bayer CropScience AG, Report No.: RAFNY002, Edition Number: M-277098-01-1 Date: 31.08.2006 GLP, unpublished Yes BCS

KIIA 6.3.2.5 /01 Moiser, D. G. 2006 BYI08330 150 OD and BYI08330 240 SC - Magnitude of the residue on potato Bayer CropScience, Stilwell, KS, USA Bayer CropScience AG, Report No.: RAFNY028, Edition Number: M-277033-01-1 Date: 25.08.2006 GLP, unpublished Yes BCS

KIIA 6.3.2.6 /01 Beedle, E. C. 2006 BYI08330 150 OD and BYI08330 240 SC - Magnitude of the residue on citrus (crop group 10, citrus fruits; includes residue reduction information) Bayer CropScience, Stilwell, KS, USA Bayer CropScience AG, Report No.: RAFNY008, Edition Number: M-277116-01-1 Date: 31.08.2006 GLP, unpublished Yes BCS

KIIA 6.3.2.7 /01 Mosier, D. G. 2006 BYI08330 150 OD and BYI08330 240 SC - Magnitude of the residue in/on grapes Englar Food Laboratories Inc., Moses Lake, WA, USA Bayer CropScience AG, Report No.: RAFNY011, Edition Number: M-277324-01-1 Date: 06.09.2006 GLP, unpublished Yes BCS

KIIA 6.3.2.8 /01 Harbin, A. M. 2006 BYI08330 150 OD and BYI08330 240 SC - Magnitude of the residue on hops Bayer CropScience, Stilwell, KS, USA Bayer CropScience AG, Report No.: RAFNY022, Edition Number: M-277130-01-1 Date: 31.08.2006 GLP, unpublished Yes BCS

KIIA 6.3.2.9 /01 Krolski, M. E. 2006 BYI08330 150 OD and BYI08330 240 SC - Magnitude of the residue on pome fruit (apple and pear) Bayer CropScience, Stilwell, KS, USA Bayer CropScience AG, Report No.: RAFNY009, Edition Number: M-277124-01-1 Date: 01.09.2006 GLP, unpublished Yes BCS

### - 241 -

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.4.1 /01 Lenz, C. A. 2006 BYI08330 - request for waiver of the requirements for poultry feeding study and analytical method for the determination of BYI08330 residues in poultry meat and eggs Bayer CropScience, Stilwell, KS, USA Bayer CropScience AG, Report No.: RAFNPO11, Edition Number: M-276816-01-1 Date: 25.07.2006 Non GLP, unpublished Yes BCS

KIIA 6.4.2 /01 Mackie, S. J. W. 2006 BYI08330 150 OD - Magnitude of the residue lactating cows Bayer CropScience, Stilwell, KS, USA Bayer CropScience AG, Report No.: RAFNX014, Edition Number: M-276834-01-1 Date: 24.08.2006 GLP, unpublished Yes BCS

KIIA 6.5.1 /01 Koch, B.; Sur,

R. 2005 BYI 08330: Aqueous hydrolysis under conditions of processing studies Bayer CropScience AG, Report No.: MEF-04/562, Edition Number: M-269158-02-1 Date: 27.09.2005, Amended: 05.04.2006 GLP, unpublished Yes BCS

KIIA 6.5.1 /02 Koch, B.; Sur,

R. 2006 BYI 08330-enol: Aqueous hydrolysis under conditions of processing studies Bayer CropScience AG, Report No.: MEF-05/227, Edition Number: M-267011-01-1 Date: 11.01.2006 GLP, unpublished Yes BCS

KIIA 6.5.1 /03 Koch, B.; Sur,

R. 2005 BYI 08330-enol-glucoside: Aqueous hydrolysis under conditions of processing studies Bayer CropScience AG, Report No.: MEF-05/274, Edition Number: M-266907-01-1 Date: 16.12.2005 GLP, unpublished Yes BCS

KIIA 6.5.1 /04 Koch, B.; Sur,

R. 2006 BYI 08330-keto-hydroxy: Aqueous hydrolysis under conditions of processing studies Bayer CropScience AG, Report No.: MEF-05/409, Edition Number: M-267024-01-1 Date: 11.01.2006 GLP, unpublished Yes BCS

KIIA 6.5.1 /05 Koch, B.; Sur,

R. 2006 BYI 08330-mono-hydroxy: Aqueous hydrolysis under conditions of processing studies Bayer CropScience AG, Report No.: MEF-05/418, Edition Number: M-267165-01-1 Date: 11.01.2006 GLP, unpublished Yes BCS

### - 242 -

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.5.3.1 /01 Schoening, R.;

Helfrich, P. 2005 Determination of the residues of BYI 08330 in/on orange fruit and the processed fractions (pulp; peel; raw juice; juice; pomace, wet; washings; fruit, washed; marmalade; peel, washed; fruit, peeled; strain, rest; peel, dried; pomace,....... Bayer CropScience AG, Report No.: RA-3032/04, Report includes Trial Nos.: 0139-04 0141-04 0239-04 0240-04 R 2004 0139/6 R 2004 0141/8 R 2004 0239/2 R 2004 0240/6 Edition Number: M-263630-01-1 Date: 21.12.2005 GLP, unpublished Yes BCS

KIIA 6.5.3.2 /01 Schoening, R.;

Helfrich, P. 2005 Determination of the residues of BYI 08330 in/on apple fruit and the processed fractions (fruit, washed; washings; strain rest; raw sauce; sauce; raw juice; juice; pomace, dried) after spraying of BYI 08330 (100 OD) in the field in......... Bayer CropScience AG, Report No.: RA-3135/04, Report includes Trial Nos.: 0795-04 0797-04 R 2004 0795/5 R 2004 0797/1 Edition Number: M-262624-02-1 Date: 15.12.2005, Amended: 12.01.2006 GLP, unpublished Yes BCS

KIIA 6.5.3.2 /02 Schoening, R.;

Helfrich, P. 2006 Determination of the residues of BYI 08330 in/on apple fruit and the processed fractions (fruit, washed; washings; strain rest; raw sauce; sauce; raw juice; juice; etc.) after spraying of BYI 08330 (100 OD) in the field in Italy and Spain Bayer CropScience AG, Report No.: RA-3137/04, Report includes Trial Nos.: 0805 - 04 0807 - 04 R 2004 0805/6 R 2004 0807/2 Edition Number: M-264335-01-1 Date: 18.01.2006 GLP, unpublished Yes BCS

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Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.5.3.3 /01 Schoening, R.;

Billian, P:; Behn, U.; Wolters, A. 2006 Determination of the residues of BYI 08330 in/on sweet cherry fruit and the processed fractions (fruit, washed; washings; fruit, depitted; preserve) and sour cherry fruit and the processed fractions (fruit, washed; washings; fruit,......... Bayer CropScience AG, Report No.: RA-3119/04, Report includes Trial Nos.: 0718-04 0720-04 0721-04 0723-04 R 2004 0718/1 R 2004 0720/3 R 2004 0721/1 R 2004 0723/8 Edition Number: M-263882-01-1 Date: 12.01.2006 GLP, unpublished Yes BCS

KIIA 6.5.3.4 /01 Ballesteros, C.;

Eberhardt, R. 2006 Determination of the residues of BYI 08330 in the processed fractions of grape, bunch of grapes for processing (raisin waste; washings; raisin) after spraying of BYI 08330 (150 OD) in the field in Spain and Italy Bayer CropScience SA, Lyon, France Bayer CropScience AG, Report No.: RA-3034/05, Report includes Trial Nos.: R20050157/9=0157-05 R20050158/7=0158-05 Edition Number: M-271371-02-1 Date: 16.05.2006, Amended: 21.08.2006 GLP, unpublished Yes BCS

KIIA 6.5.3.4 /02 Schoening, R.;

Wolters, A. 2006 Determination of the residues of BYI 08330 in/on grape (bunch of grapes) and the processed fractions (pomace, grape; must; wine) after spraying of BYI 08330 (100 OD) in the field in Germany Bayer CropScience AG, Report No.: RA-3048/04, Report includes Trial Nos.: 0192-04 0193-04 R 2004 0192/2 R 2004 0193/0 Edition Number: M-264728-01-1 Date: 26.01.2006 GLP, unpublished Yes BCS

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.5.3.4 /03 Schoening, R.;

Eberhardt, R. 2006 Determination of the residues of BYI 08330 in/on grape bunch of grapes and the processed fractions (pomace, grape; must; wine) after spraying of BYI 08330 (100 OD) in the field in Italy Bayer CropScience AG, Report No.: RA-3049/04, Report includes Trial Nos.: 0196-04 0197-04 R 2004 0196/5 R 2004 0197/3 Edition Number: M-263874-02-1 Date: 12.01.2006, Amended: 06.03.2006 GLP, unpublished Yes BCS

KIIA 6.5.3.5 /01 Freitag, T.;

Helfrich, P. 2005 Determination of the residues of BYI 08330 in/on tomato fruit and the processed fractions (washings; fruit, peeled; raw juice; juice; strain rest; preserve; puree; fruit, washed; raw puree; peel, washed; peeling water) after spraying....... Bayer CropScience AG, Report No.: RA-3140/04, Report includes Trial Nos.: 0827-04 0828-04 0829-04 0830-04 R 2004 0827/7 R 2004 0828/5 R 2004 0829/3 R 2004 0830/7 Edition Number: M-263490-01-1 Date: 20.12.2005 GLP, unpublished Yes BCS

KIIA 6.5.3.6 /01 Schoening, R.;

Billian, P.; Wolters, A. 2006 Determination of the residues of BYI 08330 in/on climbing french bean (bean with pod) and the processed fractions (washings; cooking water; bean, cooked; bean with pod, washed) after spraying of BYI 08330 (100 OD) in the greenhouse........ Bayer CropScience AG, Report No.: RA-3042/04, Report includes Trial Nos.: 0172-04 0173-04 0174-04 0175-04 R 2004 0172/8 R 2004 0173/6 R 2004 0174/4 R 2004 0175/2 Edition Number: M-263683-01-1 Date: 11.01.2006 GLP, unpublished Yes BCS

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.5.3.7 /01 Schoening, R.;

Billian, P.; Helfrich, P. 2006 Determination of the residues of BYI 08330 in/on hop cone, green, for processing and the processed fractions (cone, kiln-dried; beer; hops draff; brewer’s yeast; brewer’s malt) after spraying of BYI 08330 (100 OD) in the field in........ Bayer CropScience AG, Report No.: RA-3036/04, Report includes Trial Nos.: 0148-04 0149-04 0150-04 0151-04 R 2004 0148/5 R 2004 0149/3 R 2004 0150/7 R 2004 0151/5 Edition Number: M-265067-01-2 Date: 27.01.2006 GLP, unpublished Yes BCS

KIIA 6.5.4.1 /01 Mackie, S. J. W. 2006 BYI08330 150 OD - Magnitude of the residue on apple processed commodities Bayer CropScience, Stilwell, KS, USA Bayer CropScience AG, Report No.: RAFNY014, Edition Number: M-276832-01-1 Date: 24.08.2006 GLP, unpublished Yes BCS

KIIA 6.5.4.2 /01 Lenz, C. A. 2006 Amended report - BYI08330 150 OD - Magnitude of the residue on citrus processed commodities Bayer CropScience, Stilwell, KS, USA Bayer CropScience AG, Report No.: RAFNY016, Edition Number: M-277028-01-1 Date: 29.08.2006 GLP, unpublished Yes BCS

KIIA 6.5.4.2 /02 Krolski, M. E. 2006 BYI08330 100 OD - Reduction of the residue in grapefruit from commercial washing, waxing, and packing procedures Bayer CropScience, Stilwell, KS, USA Bayer CropScience AG, Report No.: RAFN042, Edition Number: M-276675-01-1 Date: 08.08.2006 GLP, unpublished Yes BCS

KIIA 6.5.4.3 /01 Mosier, D. G. 2006 BYI08330 150 OD - Magnitude of th e residue in/on grapes processed commodities Englar Food Laboratories Inc., Moses Lake, WA, USA Bayer CropScience AG, Report No.: RAFNY015, Edition Number: M-277287-01-1 Date: 06.09.2006 GLP, unpublished Yes BCS

### - 246 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Annex point/ reference number Author(s) Year Title Source (where different from company)

Company, Report No GLP or GEP status (where relevant)

Published or not Data Protection Claimed

Y/N-R/NR Owner

KIIA 6.5.4.4 /01 Mackie, S. J. W. 2006 BYI08330 150 OD - Magnitude of the residue on plum processed commodities Bayer CropScience, Stilwell, KS, USA Bayer CropScience AG, Report No.: RAFNY018, Edition Number: M-276380-01-1 Date: 03.02.2006 GLP, unpublished Yes BCS

KIIA 6.5.4.5 /01 Lenz, C. A. 2006 BYI08330 150 OD - Magnitude of the residue on potato processed commodities Bayer CropScience, Stilwell, KS, USA Bayer CropScience AG, Report No.: RAFNY020, Edition Number: M-276828-01-1 Date: 24.08.2006 GLP, unpublished Yes BCS

KIIA 6.5.4.6 /01 Mackie, S. J. W. 2006 BYI08330 100 OD - Magnitude of the residue on tomato processed commodities Bayer CropScience, Stilwell, KS, USA Bayer CropScience AG, Report No.: RAFNY013, Edition Number: M-277034-01-1 Date: 24.08.2006 GLP, unpublished Yes BCS

KIIA 6.6.2 /01 Sur, R.; Spiegel,

K. 2006 Metabolism of [azaspirodecenyl-3-14C]BYI 08330 in confined rotational crops Bayer CropScience AG, Report No.: MEF-05/288, Edition Number: M-269589-02-2 Date: 22.03.2006, Amended: 26.09.2006 GLP, unpublished Yes BCS

KIIA 6.6.3 /01 Lemke, V. J. 2006 BYI08330 150 OD and BYI 08330 240 SC - Magnitude of the residue in field rotational crops (limited) Bayer CropScience, Stilwell, KS, USA Bayer CropScience AG, Report No.: RAFNY019, Edition Number: M-277284-01-1 Date: 01.09.2006 GLP, unpublished Yes BCS

Annex III Data and Information

---- 247 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Annex I a: Summary of trial information – citrus fruitsApplication rateper treatmentResidues**[mg/kg]*Report No.LocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enolGlcTotal asBYI08330PHI[days]RemarksRA-2032/04R 2004 0139/6I-95044Mineo, ItalyOranges /TaroccoGallo1. 01.01.19962. 20.05.20043. 01-31.03.20050.21120.2112220022000.0100.01027.12.200417.01.2005BBCH 87 FruitFruitFruitFruitPulpPeelFruitPulpPeelFruitPulpPeel0.010.120.030.02<0.010.050.02<0.010.03<0.01<0.010.010.0120.0120.0120.012<0.0120.0580.012<0.0120.037<0.012<0.0120.0270.0120.0120.0120.012<0.0120.0300.012<0.0120.026<0.012<0.0120.024<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.0080.008<0.008<0.0080.008<0.008<0.0080.0080.0540.1640.0740.0640.0540.1580.0640.0540.1130.0540.0540.0810*07141414212121282828formulation:100 ODRA-2032/04R 2004 0141/8I-95100Catania, ItalyOranges /TaroccoGallo1. 19952. 15.04.20043. 01.01 –28.02.20050.23000.2300240024000.0100.01006.12.200427.12.2004BBCH 88 FruitFruitFruitFruitPulpPeelFruitPulpPeel<0.010.110.020.02<0.010.020.01<0.010.010.0120.0180.0170.014<0.0120.0590.012<0.0120.0250.0120.0120.0120.012<0.0120.0180.012<0.0120.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.0080.008<0.008<0.0080.0080.0540.160.0690.0660.0540.1170.0540.0540.0670*014212121282828formulation:100 ODRA-2032/04R 2004 0239/2P/2950Palmela,PortugalOranges /Dalmau1. 15.03.19802. 15.03.20043. 01.12.2004- 15.01.20050.28800.2880300030000.0100.01026.10.200416.11.2004BBCH 83 FruitFruitFruitFruitPulpPeelFruitPulpPeelFruitPulpPeel<0.010.130.130.04<0.010.040.02<0.010.020.01<0.010.01<0.0120.0230.0440.0410.0150.110.031<0.0120.0490.0330.0150.030<0.012<0.0120.0140.013<0.0120.0320.013<0.0120.0260.013<0.0120.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.0080.008<0.0080.0080.008<0.0080.0080.008<0.0080.0080.0540.1850.2080.1140.0570.2020.0840.0540.1150.0760.0570.0720*07141414212121272727formulation:100 OD- 248 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.LocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enolGlcTotal asBYI08330PHI[days]RemarksRA-2032/04R 2004 0240/6E-46450Benifaió,SpainOranges /Navelina1. 20.03.19842. 10.04.20043. 15.10.-30.11.20040.28800.2880300030000.0100.01027.09.200418.10.2004BBCH 81 FruitFruitFruitFruitPulpPeelFruitPulpPeel0.070.140.100.08<0.010.140.05<0.010.140.0520.0620.0900.0780.0630.280.0640,0560.20<0.0120.0120.0150.012<0.0120.0350.012<0.0120.033<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0110.0120.0160,0160.0080.0540,0170.0080.0520.1570.2380.2330.1980.1050.5210.1550.0980.4370*015212121282828formulation:100 ODRA-2003/05R 2005 0046/7P-2950Palmela,PortugalOrange /Dalmau1. 15.03.19802. 25.03.20053. 05.12.2005- 15.01.20060.28800.2880300030000.0100.01025.10.200515.11.2005BBCH 89 FruitFruitPulpPeelFruitPulpPeelFruitPulpPeel0.100.01<0.010.02<0.01<0.010.010.02<0.010.010.0200.015<0.0120.031<0.012<0.0120.0320.012<0.0120.0290.0120.012<0.0120.016<0.012<0.0120.0150.012<0.0120.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.0080.008<0.008<0.0080.0080.008<0.0080.0080.1520.0570.0540.0870.0540.0540.0770.0640.0540.0710141414212121282828formulation:150 ODRA-2003/05R 2005 0047/5I-96013Carlentini,ItalyOrange /TaroccoNucellare1. 19802. 15.04.20053. 01.01. -28.02.20060.28800.2880300030000.0100.01015.12.200504.01.2006BBCH 85 FruitFruitPulpPeelFruitPulpPeelFruitPulpPeel0.200.01<0.010.030.02<0.010.05<0.01<0.010.020.0130.012<0.0120.0440.012<0.0120.044<0.012<0.0120.0300.012<0.012<0.0120.0160.012<0.0120.017<0.012<0.0120.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.0080.008<0.008<0.0080.008<0.008<0.0080.0080.2450.0540.0540.110.0640.0540.1310.0540.0540.0820141414212121282828formulation:150 ODRA-2003/05R 2005 0048/3E-46400Cullera, SpainOrange/Navelina1. 25.03.19952. 05.03.20053. 10.12.20050.28800.2880300030000.0100.01005.10.200526.10.2005BBCH 81 FruitFruitFruitFruitPulpPeelFruit0.020.100.060.05<0.010.210.020.0360.0470.0490.0390.0340.200.0380.0120.0120.0240.013<0.0120.0690.013<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0080.0080.0080.0080.0080.0230.0080.0880.1790.1530.1220.0760.5140.0910*0714141421formulation:150 OD- 249 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.LocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enolGlcTotal asBYI08330PHI[days]RemarksPulpPeelFruitPulpPeel<0.010.040.01<0.010.010.0250.0980.0320.0220.072<0.0120.0440.012<0.0120.027<0.012<0.012<0.012<0.012<0.0120.0080.0160.0080.0080.0140.0670.210.0740.0640.1352121282828RA-2003/05R 2005 0049/1I-95100Catania, ItalyOrangeTaroccoGalici1. 19952. 15.04.20053. 01.01. -28.02.20060.25920.2592270027000.0100.01015.12.200504.01.2006BBCH 85 FruitFruitFruitFruitPulpPeelFruitPulpPeelFruitPulpPeel0.040.110.040.03<0.010.060.02<0.010.050.02<0.010.040.0120.0120.0140.015<0.0120.0900.016<0.0120.0590.013<0.0120.0650.0130.0120.0120.012<0.0120.0420.012<0.0120.0290.012<0.0120.035<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.0080.008<0.008<0.0080.008<0.008<0.0080.0080.0850.1540.0860.0770.0540.2120.0680.0540.1580.0650.0540.160*07141414212121282828formulation:150 ODRA-2033/04R 2004 0142/6I-Misterbianco,ItalyManderin /Clementine Nules1. 19852. 15.04.20043. 01.11.-30.12.20040.2110.211220022000.0100.01019.10.200409.11.2004BBCH 81 FruitFruitFruitFruitPulpPeelFruitPulpPeelFruitPulpPeel0.020.210.020.01<0.010.030.02<0.010.030.01<0.010.010.0730.130.120.0750.0450.240.0760.0530.210.0690.0350.110.0150.0230.0260.019<0.0120.0860.023<0.0120.0800.017<0.0120.044<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0100.0120.0150.0140.0080.0480.0150.0080.0610.0180.0080.0440.130.3870.1930.130.0870.4160.1460.0950.3930.1260.0770.220*07141414212121282828formulation:100 OD- 250 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.LocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enolGlcTotal asBYI08330PHI[days]RemarksRA-2033/04R 2004 0143/4P-Chamusca,PortugalManderin /Tangera1. 15.03.19862. 30.03.20043. 01.11.-28.11.20040.2880.288300030000.0100.01023.09.200414.10.2004BBCH 81 FruitPulpPeelFruitPulpPeelFruitPulpPeel0.01<0.010.020.01<0.010.020.01<0.010.020.150.0720.210.140.0770.180.100.0620.13<0.012<0.0120.031<0.012<0.0120.026<0.012<0.0120.016<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0290.0080.0750.0350.0080.0810.0320.0080.0730.2130.1140.3480.2090.1190.3190.1660.1040.251151515212121292929formulation:100 ODRA-2033/04R 2004 0237/6E-46400Cullera, SpainManderin /Satsuma1. 19772. 10.03.20043. 20.10-22.10.20040.2400.240250025000.0100.01022.09.200413.10.2004BBCH 79 FruitFruitFruitPulpPeelFruitPulpPeelFruitPulpPeel0.030.200.09<0.010.290.06<0.010.160.03<0.010.070.0700.120.150.0600.430.130.0540.340.120.0680.200.0190.0260.0350.0120.140.036<0.0120.120.0260.0120.068<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0200.0230.0440.0110.120.0470.0110.120.0500.0150.100.1510.3810.3310.1050.9920.2850.0990.7520.2380.1170.450*0141414212121292929formulation:100 ODRA-2033/04R 2004 0238/4E-41310Brenes, SpainMandarin /Clemenules1. 15.06.19942. 30.03.20043. 20.10-15.12.20040.2400.240250025000.0100.01027.09.200418.10.2004BBCH 81 FruitFruitFruitFruitPulpPeelFruitPulpPeelFruitPulpPeel0.030.190.010.01<0.010.010.01<0.010.010.01<0.010.010.0660.0980.0880.0660.0450.140.0690.0340.110.0750.0220.0710.0150.0160.0180.013<0.0120.0570.012<0.0120.0520.013<0.0120.038<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0180.0160.0180.0160.0080.0680.0210.0080.0650.0300.0080.0550.1410.3320.1460.1170.0870.2870.1240.0760.2490.140.0640.1860*07151515212121282828formulation:100 OD- 251 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.LocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enolGlcTotal asBYI08330PHI[days]RemarksRA-2002/05R 2005 0041/6P-2950Palmela,PortugalMandarin /Tangerinade Setúbal1. 15.02.19842. 15.03.20053. 01.12.2005– 10.01.20060.2880.288300030000.0100.01025.10.200515.11.2005BBCH 85 FruitFruitPulpPeelFruitPulpPeelFruitPulpPeel0.180.01<0.010.020.01<0.010.020.01<0.010.030.0840.0590.0320.140.0450.0290.110.0460.0320.0940.0120.012<0.0120.0260.012<0.0120.0260.012<0.0120.030<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0080.008<0.0080.0190.008<0.0080.0200.008<0.0080.0260.2960.1010.0740.2170.0870.0710.1880.0880.0740.1920141414212121282828formulation:150 ODRA-2002/05R 2005 0042/4E-46197Alfarp, SpainMandarin /Arrufatina1. 20.01.19942. 01.04.20053. 15.10.–15.11.20050.2400.240250025000.0100.01014.09.200505.10.2005BBCH 81 FruitFruitPulpPeelFruitPulpPeelFruitPulpPeel0.110.070.010.230.04<0.010.140.06<0.010.090.0780.160.0980.570.120.0830.300.120.100.330.0120.0130.0120.0670.012<0.0120.0400.0140.0120.051<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0080.0180.0080.0640.0180.0080.0550.0250.0120.0850.220.2730.140.9430.2020.1250.5470.2310.1460.5680141414212121282828formulation:150 ODRA-2002/05R 2005 0043/2I-97019Vittoria, ItalyMandarin /Tardivo diCiaculli1. 19962. 10.04.20053. 20.01.–25.02.20060.1920.192200020000.0100.01021.12.200511.01.2006BBCH 85 FruitFruitPulpPeelFruitPulpPeelFruitPulpPeel0.150.10<0.010.240.02<0.010.040.02<0.010.040.0220.033<0.0120.160.031<0.0120.100.034<0.0120.0870.0130.032<0.0120.110.015<0.0120.0640.018<0.0120.046<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0080.008<0.0080.0120.008<0.0080.0150.008<0.0080.0160.2050.1850.0540.5340.0860.0540.2310.0920.0540.2010141414212121282828formulation:BYI 08330150 OD- 252 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.LocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enolGlcTotal asBYI08330PHI[days]RemarksRA-2002/05R 2005 0044/0E-46400Cullera, SpainMandarin /Satsuma1. 30.04.19772. 01.03.20053. 07.12.20050.2400.240250025000.0100.01005.10.200526.10.2005BBCH 81 FruitFruitFruitFruitPulpPeelFruitPulpPeelFruitPulpPeel0.030.230.140.12<0.010.250.03<0.010.070.01<0.010.030.0400.0860.0920.0570.0220.220.0730.0280.180.0610.0250.130.0130.0190.0420.0310.0120.120.0280.0120.100.021<0.0120.077<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0090.100.0180.0120.0080.0540.0200.0080.0580.0180.0080.0530.1040.4470.3040.2320.0640.6560.1630.070.420.1220.0670.3020*07141414212121282828formulation:150 ODRA-2002/05R 2005 0045/9I-95045Misterbianco,ItalyMandarin /Clementine Nules1. 19852. 15.04.20053. 01.11.–31.12.20050.23040.2304240024000.0100.01017.10.200507.11.2005BBCH 81 FruitFruitFruitFruitPulpPeelFruitPulpPeelFruitPulpPeel0.020.190.060.04<0.010.060.04<0.010.100.03<0.010.060.0410.0720.0750.0660.0160.200.0690.0220.230.0680.0230.160.0120.0210.0360.033<0.0120.110.034<0.0120.140.036<0.0120.096<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0080.0110.0080.014<0.0080.0430.0180.0080.0640.0220.0080.0650.0930.3060.1910.1650.0580.4250.1730.0640.5460.1680.0650.3930*07141414212121282828formulation:150 OD* before the last treatment** Residues of each analyte calculated as spirotetramat (BYI 08330)CH Canopy height- 253 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Annex I b: Summary of trial information - lettuceApplication rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksGreenhouse trialsRA-2054/04R 2004 0393/3D-40764Langenfeld,GermanyLettuce /Alexandria(Butterheadvariety)1. 22.04.20043. 15.06.20040.0720.0720.0726006006000.0120.0120.01218.05.200425.04.200401.06.2004BBCH 47 headheadheadheadheadhead0.040.350.380.280.020.010.0960.350.270.250.0910.0530.0310.0760.0430.0610.0390.013<0.012<0.012<0.012<0.012<0.012<0.0120.0300.0370.0370.0520.0600.0810.2090.8250.7420.6550.2220.1690*013713formulation:100 ODRA-2054/04R 2004 0394/1F-31790 St.Jory, SouthernFranceLettuce /Alexandria(Butterheadvariety)1. 24.03.20043. 15.05.20040.0720.0720.0721000100010000.0070.0070.00729.04.200405.05.200412.05.2004BBCH 48 headheadheadheadheadhead0.070.490.630.060.020.010.120.690.320.180.0800.0310.0410.160.0900.0470.0250.012<0.012<0.012<0.012<0.012<0.012<0.0120.0220.0420.0270.0380.0590.0670.2651.3941.0790.3370.1960.1320*013714formulation:100 ODRA-2054/04R 2004 0396/8D-42799Leichlingen,GermanyLettuce /Roderik(Butterheadvariety)1. 02.02.20043. 15.04.20040.0720.0720.0726006006000.0120.0120.01230.03.200406.04.200413.04.2004BBCH 47 headheadheadhead2.21.71.51.90.660.500.540.590.0790.0590.0700.079<0.012<0.012<0.012<0.0120.0140.0120.0170.0322.9652.2832.1392.6130136formulation:100 ODRA-2054/04R 2004 0397/6I-00050PalidoroFiumicino,ItalyLettuce /Kereon(Butterheadvariety)1. 11.03.20043. 26.04.20040.0720.0720.0725005005000.0140.0140.01409.04.200416.04.200423.04.2004BBCH 48 headheadheadhead1.91.71.31.20.350.370.280.210.0700.0720.0460.032<0.012<0.012<0.012<0.0120.0370.0420.0430.0482.3692.1961.6811.5020137formulation:100 ODRA-2054/04R 2004 0398/4I-70043Monopoli, ItalyLettuce /Lollo rosso(Loose-Leafvariety)1. 11.10.20043. 05.01-18.01.20050.0720.0720.0728008008000.0090.0090.00922.12.200429.12.200405.01.2005BBCH 43 headheadheadheadheadhead1.75.95.13.72.60.600.490.730.680.760.530.240.130.140.140.170.150.079<0.012<0.012<0.012<0.012<0.012<0.0120.0510.0560.0520.130.150.0932.3836.8385.9844.7723.4421.0240*013614formulation:100 OD- 254 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2054/04R 2004 0399/2E-08410Bigues, SpainLettuce /Baravia(Loose-Leafvariety)1. 20.01.20043. 15.03.20040.07200.07740.072080086010000.0090.0090.00723.02.200401.03.200408.03.2004BBCH 46– 49headheadheadheadheadhead0.541.41.20.730.520.390.520.750.710.600.510.220.180.240.220.220.170.081<0.012<0.012<0.012<0.012<0.012<0.0120.0570.0580.0710.0670.0840.0741.3092.462.2131.6291.2960.7770*013714formulation:100 ODRA-2054/04R 2004 0401/8I-70043Monopoli, ItalyLettuce /Versai RZ(Loose-Leafvariety)1. 28.12.20033. 15.03.20040.0720.0720.0728008008000.0090.0090.00927.02.200405.03.200412.03.2004BBCH 49 headheadheadhead2.21.11.41.00.550.350.310.270.180.110.0930.096<0.012<0.012<0.012<0.0120.0560.0370.0490.0672.9981.6091.8641.4450137formulation:100 ODRA-2054/04R 2004 0402/6E-41310Brenes, SpainLettuce /Solsun(Nun 8801LT)(Loose-Leafvariety)1. 19.10.20043. 01.12.2004– 28.02.20050.0720.0720.0726006006000.0120.0120.01227.12.200403.01.200510.01.2005BBCH 47 headheadheadhead2.81.92.61.70.250.200.310.200.0410.0350.0520.038<0.012<0.012<0.012<0.012<0.008<0.008<0.0080.0083.1112.1552.9821.9580137formulation:100 ODRA-2170/05R 2005 1023/3GR-19007Kato Souli,GreeceLettuce /Manita1. 11.09.-10.10.20053. 21.-22.12.20050.0720.0725005000.0140.01424.11.200508.12.2005BBCH 45 headheadheadheadheadhead0.101.51.61.40.700.580.120.310.370.400.260.280.0260.0390.0570.0630.0530.053<0.012<0.012<0.012<0.012<0.012<0.0120.0270.0250.0330.0340.0320.0460.2851.8862.0721.9091.0570.9710*013714formulation:150 ODRA-2170/05R 2005 1024/1F-86380Quyilly,FranceLettuce /Bastille1. 15.09.20053. 29.10.-10.11.20050.0720.0728008000.0090.00910.10.200524.10.2005BBCH 48 headheadheadheadheadhead0.112.02.11.60.190.090.0380.570.160.180.0780.0230.0630.110.150.170.0840.052<0.012<0.012<0.012<0.012<0.012<0.0120.0150.0220.0170.0180.0230.0130.2382.7142.4391.980.3870.190*013714formulation:150 ODRA-2170/05R 2005 1026/8NL-1852 RHHeiloo,NetherlandsLettuce /Varinka1. 14.09.-05.10.20053. 12.-15.12.20050.0720.072100010000.0070.00722.11.200506.12.2005BBCH 48 headheadheadheadheadhead0.451.61.51.41.30.870.180.340.300.290.350.260.0630.0670.0850.0820.0860.066<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0080.7132.0271.9051.7921.7561.2160*013714formulation:150 OD- 255 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2170/05R 2005 1027/6P-2560 TorresVedras,PortugalLettuce /Tradition1. 18.08.20053. 26.-27.09.20050.0720.0725005000.0140.01426.08.200509.09.2005BBCH 41 headheadheadheadheadhead<0.011.41.61.40.170.02<0.0121.00.380.330.120.043<0.0120.0670.110.0990.0340.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0080.0150.0200.0450.0380.0240.0542.4942.1221.8860.3740.1110*013714formulation:150 ODRA-2170/05R 2005 1028/4F-31790 St.Jory, FranceLettuce /Cabanon1. 20.09.20053. 05.-15.01.20060.0720.0728008000.0090.00919.12.200503.01.2006BBCH 45 headhead1.81.50.220.230.0470.081<0.012<0.0120.0080.0122.0871.83507formulation:150 ODRA-2170/05R 2005 1029/2F-84140Montfavet,FranceLettuce /Arcadia1. 20.09.-05.10.20053. 28.-29.11.20050.0720.072100010000.0070.00707.11.200521.11.2005BBCH 48 headhead1.50.850.660.410.110.12<0.012<0.0120.0150.0142.2971.40607formulation:150 ODRA-2170/05R 2005 1030/6D-40764Langenfeld,GermanyLettuce /Alexandria1. 26.07.20053. 30.08.-10.09.20050.0720.0726006000.0120.01210.08.200524.08.2005BBCH 43 headhead1.30.050.300.0560.0140.031<0.012<0.0120.0080.0141.6340.16307formulation:150 ODRA-2170/05R 2005 1031/4E-08410Bigues i Riells,SpainLettuce /Batavia1. 26.09.20053. 28.12.2005– 05.01.20060.07640.07206369000.0080.01207.12.200520.12.2005BBCH 48 headhead1.81.60.570.580.120.12<0.012<0.0120.0080.0152.512.32707formulation:150 ODRA-2113/04R 2004 0685/1D-40764Langenfeld,GermanyLettuce /Alexandria1. 22.04.20043. 15.06.20040.0720.0720.0726006006000.0120.0120.01218.05.200425.05.200401.06.2004BBCH 47 headheadheadheadheadhead0.020.420.50.310.030.010.0880.380.290.210.10.0540.0230.0930.0480.0370.0280.012<0.012<0.012<0.012<0.012<0.012<0.0120.0360.0420.0510.0560.070.0840.1790.9470.9010.6250.240.1720*013713formulation:240 SC;addition of0.2% RME500- 256 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2113/04R 2004 0687/8I-70043Monopoli, ItalyLettuce /Lollo rosso1. 11.10.20043. 05.01. –18.01.20050.0720.0720.0728008008000.0090.0090.00922.12.200429.12.200405.01.2005BBCH 43 headheadheadheadheadhead1.24.23.21.70.990.210.360.660.490.620.410.230.120.150.120.140.110.069<0.012<0.012<0.012<0.012<0.012<0.0120.0420.0430.0420.110.120.111.7345.0653.8642.5821.6420.6310*013714formulation:240 SC;addition of0.2% RME500RA-2113/04R 2004 0688/6E-41340Brenes, SpainLettuce /Solsun(Nun 8801LT)1. 19.10.20043. 01.12.2005– 28.02.20050.0720.0720.0726006006000.0120.0120.01227.12.200403.01.200510.01.2005BBCH 47 headheadheadheadhead1.11.82.21.71.50.150.210.290.180.210.0360.0320.050.0440.044<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.0081.3062.0622.561.9441.7740*0137formulation:240 SC;addition of0.2% RME500RA-2113/04R 2004 0689/4D-42799Leichlingen,GermanyLettuce /Roderick1. 02.02.20043. 15.04.20040.0720.0720.0726006006000.0120.0120.01230.03.200406.04.200413.04.2004BBCH 47 headheadheadheadhead1.22.11.81.61.50.190.280.250.270.210.0640.0810.0890.080.066<0.012<0.012<0.012<0.012<0.0120.010.0120.010.130.0191.4762.4852.1612.0921.8070*0136formulation:240 SC;addition of0.2% RME500Field conditions – Northern EuropeRA-2052/04R 2004 0385/2NL-1681 NDZwaagdijkOost,NetherlandsLettuce /Ponchito(Butterheadvariety)1. 10.06.20043. 28.07 –04.08.20040.0720.0720.0728008008000.0090.0090.00913.07.200421.07.200428.07.2004BBCH 44 headheadheadheadheadhead0.030.530.460.370.170.030.0850.150.180.20.10.0260.050.050.0570.0640.0820.019<0.012<0.012<0.012<0.012<0.012<0.0120.0330.0310.040.0570.0770.0630.210.7730.7490.7030.4410.150*013714formulation:100 ODRA-2052/04R 2004 0386/0D-40764Langenfeld,GermanyLettuce /Ponchito(Butterheadvariety)1. 22.04.20043. 15.06.20040.0720.0720.0726006006000.0120.0120.01225.05.200401.06.200408.06.2004BBCH 48 headheadheadhead0.370.390.050.010.30.240.120.0550.090.0740.0490.021<0.012<0.012<0.012<0.0120.0140.0150.0240.0190.7860.7310.2550.1170136formulation:100 ODRA-2052/04R 2004 0387/9D-53332BornheimSechten,GermanyLettuce /Lollo Roso(Loose-Leafvariety)1. 20.04.20043. 14.06. –15.06.20040.0720.0720.0726006006000.0120.0120.01218.05.200425.05.200401.06.2004BBCH 48 headheadheadheadheadhead0.241.21.20.240.090.010.140.640.460.30.130.0270.150.190.180.140.0650.018<0.012<0.012<0.012<0.012<0.012<0.0120.0250.0280.0340.0380.0440.0330.5672.071.8860.730.3410.10*013714formulation:100 OD- 257 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2052/04R 2004 0388/7D-40764Langenfeld,GermanyLettuce /Bastille(Loose-Leafvariety)1. 22.04.20043. 15.06.20040.0720.0720.0726006006000.0120.0120.01225.05.200401.06.200408.06.2004BBCH 48 headheadheadhead0.580.130.010.010.450.260.110.0680.0620.0570.0590.028<0.012<0.012<0.012<0.0120.0290.0280.0390.0331.1330.4870.230.1510136formulation:100 ODField conditions – Southern EuropeRA-2053/04R 2004 0389/5F-69480Lucenay,FranceLettuce /45091. 03.05.20043. 06.06. –22.06.20040.0720.0720.0725505505500.0130.0130.01325.05.200402.06.200408.06.2004BBCH 42 headheadheadheadheadhead0.010.010.040.020.01<0.010.0460.0540.130.0760.0430.0130.0220.0240.0340.0280.0170.012<0.012<0.012<0.012<0.012<0.012<0.0120.0110.0120.020.0240.0240.0220.1010.1120.2360.160.1060.0690*013614formulation:100 ODRA-2053/04R 2004 0390/9E-08410Vilanova delVallés, SpainLettuce /Iceberg1. 10.06.20043. 15.07. –22.07.20040.0720.0770.07260085610000.0120.0090.00701.07.200407.07.200415.07.2004BBCH 47 headheadheadhead0.740.30.20.040.280.310.130.0410.0670.0860.0730.02<0.012<0.012<0.012<0.0120.0450.0460.0530.0421.1440.7540.4680.1550137formulation:100 ODRA-2053/04R 2004 0391/7P-2665-018Azueira,PortugalLettuce /Vision1. n.r.3. n.r.0.0720.0720.0727507507500.0100.0100.01012.04.200419.04.200426.04.2004BBCH 32 headheadheadheadheadhead0.031.30.40.330.050.020.0710.520.320.190.0780.0290.0250.0560.0830.0850.0280.012<0.012<0.012<0.012<0.012<0.012<0.0120.0180.020.0210.0210.020.0140.1561.9080.8360.6380.1880.0870*013714formulation:100 ODRA-2053/04R 2004 0392/5I-40128Bologna, ItalyLettuce /Gentilina1. 18.08.20043. 01.10. –15.10.20040.0720.0720.0725005005000.0140.0140.01421.09.200428.09.200405.10.2004BBCH 49 headheadheadhead0.850.480.260.040.160.210.20.120.0390.0560.0870.035<0.012<0.012<0.012<0.0120.0370.0310.050.0581.0980.7890.6090.2650137formulation:100 OD* before the last treatment** Residues of each analyte calculated as spirotetramat (BYI 08330)n.r. not reported- 258 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Annex I c: Summary of trial information – pome fruitApplication rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksNorthern EuropeRA-2135/04R 2004 0795/5D-51399Burscheid,GermanyAppleJonagold1. 01.03.19832. 03.05.20043. 10.09.2004- 30.10.20040.14400.1440100010000.0140.01410.08.200424.08.2004BBCH 77 fruitfruitfruitfruit0.100.020.010.02<0.0120.0160.0120.0120.0120.0140.0120.017<0.012<0.012<0.0120.012< 0.008< 0.008< 0.0080.0080.1440.0700.0540.0690132127formulation:100 ODRA-2135/04R 2004 0796/3D-51399Burscheid,GermanyPearVereinsdechantbirne1. 01.03.19862. 20.04.20043. 01.09.2004- 30.10.20040.14400.1440100010000.0140.01410.08.200424.08.2004BBCH 77 fruitfruitfruitfruit0.150.020.020.010.012<0.012<0.012<0.0120.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.0080.1940.0640.064<0.0540132127formulation:100 ODRA-2135/04R 2004 0797/1GB-SG8 8SSRoyston,UnitedKingdomAppleJonathan1. 19942. 12.04.20043. 01.10.2004- 01.11.20040.13700.13709509500.0140.01408.09.200424.09.2004BBCH 85 fruitfruitfruitfruitfruitfruit0.070.210.120.070.040.020.0140.0170.0250.0260.0340.0330.0120.0120.0180.0130.0210.025<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0080.1160.2590.1830.1290.1150.098007132128formulation:100 ODRA-2135/04R 2004 0799/8F-78920ECQUEVILLY,N-FrancePearConference1. 25.09.19602. 10.04.20043. 07.09.2004- 15.09.20040.14400.14406006000.0240.02406.08.200421.08.2004BBCH 78 fruitfruitfruitfruitfruitfruit0.030.140.060.060.050.03<0.0120.0120.0120.0120.012<0.012<0.012<0.0120.0120.0120.0120.0120.0120.0120.0120.0120.0120.012<0.008<0.008<0.008<0.008<0.008<0.0080.0740.1840.1040.1040.0940.074006132127formulation:100 ODRA-2012/05R 2005 0083/1GB-CO6 5LEEssex, UKapple /Cox1. 19952. 25.04.20053. 19.09 –17.10.20050.1440.144100010000.0140.01431.08.200514.09.2005BBCH 85 fruitleafleafleaffruitleaffruitfruit0.119.56.25.50.053.20.030.010.0230.770.350.60.0310.170.0340.0210.0120.591.11.10.0141.30.0150.019<0.0120.0120.0120.012<0.0120.012<0.012<0.012<0.0080.0080.0080.01<0.0080.011<0.008<0.0080.16510.887.677.2220.1154.6930.0990.07003614142129formulation:150 OD- 259 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2012/05R 2005 0085/8GB-CB4 5HGCambgidge,UKpear /Conference1. 19882. 10.04.20053. 05.09 –23.09.20050.1440.144100010000.0140.01416.08.200530.08.2005BBCH 81 fruitleafleafleaffruitleaffruitfruit0.3824195.40.083.50.050.040.0241.50.560.240.0120.130.0120.0120.0120.370.970.450.0220.370.0160.0120.0120.0370.0720.0840.0120.0830.0120.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.0080.43625.91520.616.1820.1344.0910.0980.084003714142128formulation:150 ODRA-2012/05R 2005 0086/6D-88069Bernau,Germanyapple /Jonagold1. 01.03.19932. 30.04.20053. 21.09 –24.10.20050.18720.1872130013000.0140.01417.08.200531.08.2005BBCH 85 fruitfruitleafleaffruitleaffruitleaffruitfruit0.020.12139.60.107.20.032.20.030.020.0160.0170.790.750.0220.280.0190.0930.0210.0120.0120.0120.761.20.0151.10.0180.640.0230.017<0.012<0.0120.0190.0240.0120.0390.0120.0430.0120.012<0.008<0.0080.0080.010<0.0080.017<0.0080.0180.008<0.0080.0680.16914.57711.5840.1578.6360.0872.9940.0940.0690*0027714142128formulation:150 ODRA-2012/05R 2005 0087/4D-65366Geisenheim,Germanypear /Conference1. 15.11.19842. 13.04.20053. 05.09. –19.09.20050.1440.144100010000.0140.01404.08.200518.08.2005BBCH 81 fruitfruitleafleaffruitleaffruitleaffruitfruit0.040.2524220.22190.14130.10.060.0120.0231.50.430.0130.560.0120.440.0120.0120.0120.0120.50.780.0130.530.0170.770.0160.0140.0130.0140.230.210.020.220.0210.250.020.021<0.008<0.0080.0080.0090.0080.0080.0080.0080.008<0.0080.0850.30726.23823.4290.27420.3180.19814.4680.1560.1150*0037714142128formulation:150 ODRA-2012/05R 2005 1018/7D-4808WurzenRoitzsch,Germanyapple /Gloster1. 01.10.19892. 20.04.20053. 20.08. –24.10.20050.2160.216150015000.0140.01426.07.200508.08.2005BBCH 77 fruitfruitfruitfruit0.140.080.070.060.0220.0490.0520.0370.0120.0120.0130.012<0.0120.0120.0120.012<0.008<0.0080.0080.0080.1940.1610.1550.1290152229formulation:150 OD- 260 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2138/04R 2004 0809/9D-51399Burscheid,Germanyapple /Mutzu1. 01.03.19832. 22.04.20043. 15.10. –31.10.20040.1440.144100010000.0140.01406.09.200420.09.2004BBCH 81 fruitfruitfruitfruit0.130.010.020.01<0.0120.0120.0120.012<0.012<0.0120.0120.012<0.012<0.012<0.012<0.012<0.008<0.0080.008<0.0080.1740.0540.0640.0540142128formulation:240 SC;addition of0.2% RME500RA-2138/04R 2004 0810/2D-51399Burscheid,Germanypear /Tongern1. 01.03.19862. 20.04.20043. 15.09. –30.09.20040.1440.144100010000.0140.01410.08.200424.08.2004BBCH 77 fruitfruitfruitfruit0.180.150.140.140.0390.0340.0330.0310.0350.0330.0290.0270.0530.0460.0440.0430.0080.0080.0080.0080.3150.2710.2540.2490132127formulation:240 SCRA-2138/04R 2004 0811/0GB-SG8 8SSRoyston, UKapple /Jonathan1. 19942. 12.04.20043. 01.10. –01.11.20040.13680.13689509500.0140.01408.09.200424.09.2004BBCH 85 fruitfruitfruitfruitfruitfruit0.020.230.06<0.010.020.01<0.0120.0120.012<0.0120.0120.012<0.0120.0120.012<0.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0080.0640.2740.1040.0540.0640.0540*07132128formulation:240 SC; 2ndapplication:addition of0.2% RME500;water rate300 L/haper m CHRA-2138/04R 2004 0812/9F-78920Ecquevilly, NFrancepear /Conference1. 25.09.19602. 10.04.20043. 07.09. –15.09.20040.1440.1446006000.0240.02406.08.200421.08.2004BBCH 78 fruitfruitfruitfruitfruitfruit0.030.190.110.060.070.05<0.0120.0120.0120.0120.012<0.012<0.0120.0120.0120.0120.0120.012<0.012<0.0120.0120.0120.0120.012<0.008<0.008<0.008<0.008<0.0080.0080.0740.2340.1540.1040.1140.0940*06132127formulation:240 SC;addition of0.2% RME500Southern EuropeRA-2137/04R 2004 0805/9I-44043Mirobello, Italyapple /Nero RedRome1. 10.01.19872. 10.04.20043. 20.09. –15.10.20040.2160.216150015000.0140.01424.08.200407.09.2004BBCH 81 fruitfruitfruitfruit0.300.060.040.050.0190.0150.0140.0130.0120.0120.0120.012<0.012<0.012<0.0120.012<0.008<0.008<0.008<0.0080.3510.1070.0860.0950142128Form.: 100ODRA-2137/04R 2004 0806/4I-44040Merelli, Italypear /Abate fetel1. 10.01.19802. 20.04.20043. 25.08. –15.09.20040.2160.216150015000.0140.01406.08.200421.08.2004BBCH 79 fruitfruitfruitfruit0.270.100.070.100.0330.0120.0120.0120.020.0190.0130.019<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.0080.3430.1510.1150.1510142128formulation:100 ODRA-2137/04R 2004 0807/2E-17474apple /Golden1. 01.02.19902. 01.04.20043. 15.09. –0.2160.216150015000.0140.01405.08.200420.08.2004BBCH 81 fruitfruitfruit0.090.230.200.0130.0160.0230.0190.020.0340.0170.0160.027<0.0080.0080.0080.1470.290.2920*010formulation:100 OD- 261 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksVilamacolum,Spain20.09.2004fruitfruitfruit0.120.100.050.0220.0150.0120.0340.0410.0320.0250.0280.0210.0080.0080.0080.2090.1920.123142027RA-2137/04R 2004 0808/0F-69380 LesChères, SFrancepear –Passecrassane1. 10.01.19872. 10.04.20043. 20.09. –15.10.20040.18720.18726506500.0290.02906.08.200421.08.2004BBCH 76 fruitfruitfruitfruitfruitfruit0.120.380.180.150.140.140.0300.0630.0380.0330.0330.0320.0260.0390.0340.0310.0270.0270.0320.130.0530.0450.0410.0410.0080.0080.0080.0080.0080.0080.2160.620.3130.2670.2490.2480*07142128formulation:100 OD;water rate250 L/haper m CHRA-2015/05R 2005 0088/2F-79310SaintPardoux, SFranceapple /Braeburn1. 10.01.19852. 13.04.20053. 01.10. –31.10.20050.18720.1872130013000.0140.01409.09.200523.09.2005BBCH 81 fruitfruitfruitfruitfruitfruit0.030.110.080.040.040.030.0120.0120.0120.0130.0220.02<0.012<0.0120.0120.0120.0140.023<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0080.0740.1540.1240.0850.0960.0930*07142128formulation:150 ODRA-2015/05R 2005 0089/0I-40128Bologna, Italyapple /Jonathan1. 01.02.19882. 15.04.20053. 05.08. –15.08.20050.15840.1584110011000.0140.01405.07.200519.07.2005BBCH 78 fruitfruitfruitfruit0.110.060.080.020.0120.0120.0120.0120.0120.0120.0150.0120.0120.0120.0140.012<0.0080.0080.0080.0080.1540.1040.1290.0640142128formulation:150 ODRA-2015/05R 2005 0090/4F-31330Grenade, SFrancepear –BeurreHardy1. 01.01.19752. 25.03.20053. 18.08. –23.08.20050.18000.1800125012500.0140.01413.07.200527.07.2005BBCH 81 fruitfruitfruitfruitfruitfruit0.040.140.050.050.020.020.0120.0220.0120.0120.012<0.0120.020.0160.0290.0290.0220.018<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0080.0920.1980.1110.1110.0740.0700*07142128formulation:150 ODRA-2015/05R 2005 0091/2I-37050 AlbaroDi RoncoAll’Adige, Italypear –William1. 19952. 10.04.20053. 15.08. –25.08.20050.2160.216150015000.0140.01412.07.200526.07.2005BBCH 78 fruitfruitfruitfruit0.110.030.020.010.012<0.012<0.012<0.0120.0120.0140.014<0.012<0.012<0.0120.0120.012<0.008<0.008<0.008<0.0080.1540.0760.0660.0540142128formulation:150 ODRA-2136/04R 2004 0800/5I-44043Mirabello, Italyapple /Nero RedRome1. 10.01.19872. 10.04.20043. 20.09. –15.10.20040.2160.216150015000.0140.01424.08.200407.09.2004BBCH 81 fruitfruitfruitfruit0.350.040.010.010.0190.0120.0120.0120.0150.0120.0120.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.0080.4040.084<0.054<0.0540142128formulation:240 SC0.2 %additiveRME 500EW wasadded- 262 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2136/04R 2004 0800/5I-44040 DodiciMorelli, Italypear /Abate fetel1. 10.01.19802. 20.04.20043. 25.08. –15.09.20040.2160.216150015000.0140.01422.07.200405.08.2004BBCH 79 fruitfruitfruitfruit0.220.10.080.090.0320.0120.0120.0120.0120.0240.0180.018<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.0080.2840.1560.130.140142128formulation:240 SC;addition of0.2 % RME500 EW;water rate250 L/haper m CHRA-2136/04R 2004 0802/1E-17474Vilamacolum,Spainapple /Golden1. 01.02.19902. 01.04.20043. 15.09. –20.09.20040.2160.216150015000.0140.01405.08.200420.08.2004BBCH 81 fruitfruitfruitfruitfruitfruit0.140.330.250.110.090.050.0120.0120.0120.0130.0120.0120.0120.0120.0170.0190.0220.0140.0120.0120.0120.0120.0120.012<0.008<0.008<0.008<0.008<0.008<0.0080.1840.3740.2990.1620.1440.0960*010142027formulation:240 SCaddition of0.2 % RME500 EWRA-2136/04R 2004 0804/8F-69380 LesChères, SFrancepear –Passecrassane1. 01.01.19622. 12.04.20043. 03.09.20040.18720.18726506500.0290.02929.07.200413.08.2004BBCH 76 fruitfruitfruitfruitfruitfruit<0.010.140.02<0.010.01<0.01<0.0120.012<0.012<0.012<0.012<0.012<0.0120.0120.012<0.0120.012<0.012<0.0120.0120.012<0.0120.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0080.0540.1840.0640.054<0.054<0.0540*07142128formulation:240 SC;addition of0.14 %RME 500EW; waterrate 250L/ha per mCH* before the last treatment** Residues of each analyte calculated as spirotetramat (BYI 08330)CH Canopy height- 263 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Annex I d: Summary of trial information – Peach andapricotApplication rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksNorthern EuropeRA-2126/04R 2004 0785/8F-36300Pouligny SaintPierre, NFrancepeach /Nerine1. 19902. 15.03.20043. 05.07. –10.07.20040.18000.1800125012500.0140.01404.06.200418.06.2004BBCH 77 fruitfruitfruitfruit0.510.100.070.070.130.240.150.150.0530.0410.0290.0320.0360.0570.0530.0530.0090.0130.0120.0120.7380.4510.3140.3170142127formulation:100 ODRA-2126/04R 2004 0786/6D-65366Geisenheim,Germanyapricot /Goldrich1. 15.11.19982. 17.03.20043. 30.06. –14.07.20040.14400.1440100010000.0140.01401.06.200415.06.2004BBCH 75fruitfruitfruitfruitfruitfruit0.070.260.170.120.140.090.0740.0940.140.120.0950.0770.0190.0160.0180.0130.0140.0130.0120.0120.0120.0120.0120.0120.150.110.180.210.250.280.3250.4920.5200.4750.5110.4720*07142128formulation:100 ODRA-2006/05R 2005 0059/9D-06179Höhnstedt,Germanyapricot /Stark EarlyOrange1. 01.03.19972. 01.04.20053. 01.07. –20.07.20050.18000.1800125012500.0140.01409.06.200523.06.2005BBCH 78 fruitfruitfruit0.390.070.040.250.370.290.0580.0440.0340.0120.0120.0120.260.370.320.9700.8660.69601421formulation:150 ODRA-2006/05R 2005 0060/2D-65366Geisenheim,Germanyapricot /Goldrich1. 15.11.20002. 15.03.20053. 07.07. –21.07.20050.14400.14406006000.0240.02408.06.200522.06.2005BBCH 75 fruitfruitfruitfruitfruit0.100.290.150.080.070.0850.0920.190.210.130.0120.0120.0140.0160.0180.0120.0120.0120.0120.0120.0820.0860.170.240.290.2910.4920.5360.5580.5200*071421formulation:150 OD;water rate300 L/haper m CHRA-2006/05R 2005 0061/0F-36300Pouligny SaintPierre, NFrancepeach /Nerine1. 01.02.19922. 15.03.20053. 04.07. –15.07.20050.18000.1800125012500.0140.01402.06.200516.06.2005BBCH 78 fruitfruitfruitfruitfruitfruit0.120.260.140.100.060.040.0800.0880.250.240.250.180.0320.0320.0420.0330.0350.0270.0120.0120.0620.0740.0830.065<0.008<0.0080.0080.0090.0100.0090.2520.4000.5020.4560.4380.3210*07142127formulation:150 OD- 264 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksSouthern EuropeRA-2127/04R 2004 0787/4E-08784 LaFortesa, Spainpeach /Ruby Rich1. 19962. 22.03.20043. 23.06. –28.06.20040.18000.1800125012500.0140.01418.05.200401.06.2004BBCH 76 fruitfruitfruitfruit0.480.080.040.020.230.280.190.130.0570.0370.0270.0200.030.0920.0810.0870.0080.0080.0080.0080.8050.4970.3460.2650142227formulation:100 ODRA-2127/04R 2004 0788/2I-40128Bologna, Italyapricot /Bellad’Imola1. 10.11.20012. 01.03.20043. 26.06. –02.07.20040.18000.1800125012500.0140.01425.05.200408.06.2004BBCH 77 fruitfruitfruitfruit0.420.080.070.040.270.230.140.0860.0410.030.0230.0200.0120.0140.0160.0150.220.370.430.400.9630.7240.6790.5610142128formulation:100 ODRA-2127/04R 2004 0789/0I-48100Ravenna, Italypeach /RedHaven1. 30.11.19972. 15.03.20043. 10.07. –31.07.20040.18000.1800125012500.0140.01416.06.200430.06.2004BBCH 81 fruitfruitfruitfruitfruitfruit0.080.330.150.050.030.010.0480.0680.120.100.0710.0440.0440.0460.0500.0340.0170.0120.0230.0280.0390.0400.0440.0390.0080.0090.0090.0080.0080.0080.2030.4810.3680.2320.1700.1130*07142128formulation:100 ODRA-2127/04R 2004 0790/4E-46840Pobla del Duc,Spainapricot /Canino1. 20002. 15.02.20043. 05.06. –20.06.20040.12960.12969009000.0140.01427.04.200413.05.2004BBCH 75 fruitfruitfruitfruitfruitfruit0.010.160.070.040.020.020.0480.0740.0930.0990.130.0910.0120.0220.0230.0150.0140.012<0.012<0.012<0.012<0.0120.0120.0120.0360.0500.0730.0770.110.120.1180.3180.2710.2430.2860.2550*07142128formulation:100 ODRA-2007/05R 2005 0062/9P-2580-555Mato, Portugalapricot /Canino1. 15.01.19972. 02.04.20053. 10.06. –11.06.20050.14400.1440100010000.0140.01413.04.200527.04.2005BBCH 75 fruitfruitfruitfruit0.610.210.090.100.400.300.160.110.0940.0970.0850.0500.0120.0120.0120.0120.120.340.340.331.2360.9590.6870.6020142128formulation:150 ODRA-2007/05R 2005 0063/7E-08784 LaFortesa, Spainpeach /Richlady1. 15.01.19932. 25.03.20053. 05.07. –10.07.20050.16070.1728111612000.0140.01427.05.200510.06.2005BBCH 75 fruitfruitfruitfruit0.350.190.090.060.0620.150.0930.0710.0340.0480.0160.0120.0200.0970.100.110.0080.0080.0080.0080.4740.4930.3070.2610132028formulation:150 ODRA-2007/05R 2005 0064/5GR-20200SouliKorinthias,Greeceapricot /Bebekou1. 19942. 15.03.20053. 04.07. –14.07.20050.17280.1800120012500.0140.01431.05.200514.06.2005BBCH 75 fruitfruitfruitfruit0.250.150.050.050.0640.0940.0630.0390.0120.0120.0120.012<0.012<0.0120.012<0.0120.0460.100.0990.100.3840.3680.2360.2130142128formulation:150 OD- 265 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2007/05R 2005 0065/3F-84200Montfavet, SFrancepeach /Springwhite1. 10.03.19982. 15.03.20053. 12.06. –28.06.20050.17280.1800120012500.0140.01411.05.200525.05.2005BBCH 75 fruitfruitfruitfruitfruitfruit0.040.220.090.050.030.020.0370.0610.110.0710.0470.0540.0220.0220.0230.0140.0120.0120.0120.0120.0190.0220.0180.019<0.008<0.008<0.008<0.008<0.008<0.0080.1190.3230.250.1650.1150.1130*07142128formulation:150 ODRA-2007/05R 2005 0066/1I-40128Bologna, Italyapricot /Bella diImola1. 10.11.20012. 01.03.20053. 28.06. –02.07.20050.18000.1800125012500.0140.01424.05.200507.06.2005BBCH 79 fruitfruitfruitfruitfruitfruit0.040.120.050.030.020.020.0580.0790.140.100.0610.0400.0120.0140.0150.0120.0120.013<0.0120.0120.0120.0120.0120.0120.0640.0740.0990.110.170.160.1860.2990.3160.2640.2750.2450*07142127formulation:150 OD* before the last treatment** Residues of each analyte calculated as spirotetramat (BYI 08330)CH Canopy height- 266 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Annex I e: Summary of trial information – PlumApplication rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksNorthern EuropeRA-2124/04R 2004 0774/2D-04808WurzenRoitzsch,Germanyplum /CacaksSchöne1. 01.10.19892. 20.04.20043. 01.08. –10.09.20040.2160.216150015000.0140.01414.07.200428.07.2004BBCH 81 fruitfruitfruitfruit0.200.080.050.040.310.450.320.290.0270.0410.0310.0380.0860.250.250.330.0340.110.100.130.6570.9310.7510.8280142128formulation:100 ODRA-2124/04R 2004 0775/0D-51399Burscheid,Germanyplum /CacaksFruchtbare1. 01.03.19932. 18.04.20043. 01.08. –15.08.20040.1440.144100010000.0140.01429.06.200413.07.2004BBCH 75 fruitfruitfruitfruit0.160.020.010.010.0710.0610.0340.0150.0120.0120.0120.0120.0310.0720.0780.0840.0080.0200.0250.0240.2820.1850.1590.1450142128formulation:100 ODRA-2124/04R 2004 0776/9F-36300Pouligny St.Pierre, NFranceplum /Opale1. 19842. 30.03.20043. 15.07. –26.07.20040.1800.180125012500.0140.01414.06.200428.06.2004BBCH 77 fruitfruitfruitfruitfruitfruit0.080.370.160.090.070.060.210.220.310.250.260.260.0270.0290.0290.0250.0250.0280.0490.0530.0580.0570.0640.0840.050.0570.0780.0780.110.150.4160.7290.6350.50.5290.5820*07142128formulation:100 ODRA-2124/04R 2004 0777/7GB-CB4 5HGCambridge,UKplum /Edwards1. 19942. 11.04.20043. 22.08. –12.09.20040.1800.180125012500.0140.01428.07.200411.08.2004BBCH 81 fruitfruitfruitfruitfruitfruit0.070.250.140.100.090.070.150.150.170.170.130.140.0120.0120.0120.0150.0140.0170.0890.0850.110.130.150.200.0420.0420.0460.0550.0640.0840.3630.5390.4780.470.4480.5110*07142128formulation:100 ODRA-2004/05R 2005 0050/5GB-CB4 5HGCambridge,UKplum /Edwards1. 19892. 18.04.20053. 19.08. –09.09.20050.1800.180125012500.0140.01402.08.200516.08.2005BBCH 85 fruitfruitfruitfruit0.160.070.040.030.0920.170.190.140.0120.0120.0120.0120.0170.0370.0780.0830.0080.0150.0330.0340.2890.3040.3530.2990142128formulation:150 OD- 267 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2004/05R 2005 0051/3F-36300Pouligny St.Pierre, Franceplum /ReineClaudeVerte1. 19922. 01.04.20053. 22.07. –04.08.20050.1440.144100010000.0140.01420.06.200504.07.2005BBCH 79 fruitfruitfruitfruit0.260.060.040.030.090.0990.110.0630.0120.0120.0120.0120.0960.210.230.190.0110.0190.0240.0160.4690.4000.4160.3110142128formulation:150 ODRA-2004/05R 2005 0052/1D-40789Monheim,Germanyplum /Ersinger1. 01.04.19892. 20.04.20053. 01.07. –15.08.20050.2160.216150015000.0140.01401.06.200515.06.2005BBCH 75 fruitfruitfruitfruitfruitfruit0.010.080.050.030.020.020.0230.0440.0950.0620.0270.0430.0120.0120.0170.0150.0170.0120.0120.0120.0620.110.0980.10<0.008<0.0080.0090.0160.0160.0180.0650.1560.2330.2330.1780.1930*07142128formulation:150 ODRA-2004/05R 2005 0054/8D-04808WurzenRoitzsch,Germanyplum /CacaksSchöne1. 01.10.19962. 15.04.20053. 01.08. –05.09.20050.2160.216150015000.0140.01419.07.200502.08.2005BBCH 76 fruitfruitfruitfruitfruitfruit0.020.080.060.050.020.030.0390.0520.0820.0740.0410.0430.0120.0120.0120.0120.0120.0120.0140.0170.0190.0210.0180.0220.0080.0080.0100.0090.0100.0120.0930.1690.1830.1660.1010.1190*07142128formulation:150 ODSouthern EuropeRA-2125/04R 2004 0778/5F-31620Fronton, SFranceplum /Bave1. 19942. 15.05.20043. 05.08. –20.08.20040.2160.216150015000.0140.01408.07.200422.07.2004BBCH 79 fruitfruitfruitfruit0.150.090.060.050.120.190.160.110.0130.0210.0210.020.0730.190.20.220.0220.0430.0440.0440.3780.5340.4850.4440142128formulation:100 ODRA-2125/04R 2004 0779/3I-48100Ravenna, Italyplum /Gocciad`Oro1. 20012. 01.04.20043. 05.07. –26.07.20040.1800.180125012500.0140.01414.06.200428.06.2004BBCH 81 fruitfruitfruitfruitfruitfruit0.030.210.110.040.030.020.0930.0960.180.150.0920.060.0140.0180.0180.0160.0130.0120.0120.0120.0140.020.0230.0290.0090.0090.0140.0210.0230.0280.1580.3450.3360.2470.1810.1490*07142128formulation:100 ODRA-2005/05R 2005 0055/6I-41058Viglona, Italyplum /President1. 15.01.20012. 28.03.20053. 20.08. –10.09.20050.1440.144100010000.0140.01421.07.200504.08.2005BBCH 79 fruitfruitfruitfruit0.340.090.080.030.0550.120.0880.0370.0120.0120.0120.0120.0540.130.170.150.0180.040.0450.0360.4790.3920.3950.2650142128formulation:150 OD- 268 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2005/05R 2005 0058/0E-46840Pobla del Duc,Spainplum /Black Gold1. 01.02.19922. 20.02.20053. 10.07. –20.07.20050.1440.144100010000.0140.01406.06.200520.06.2005BBCH 77 fruitfruitfruitfruitfruitfruit0.030.120.110.070.050.030.0360.0470.0630.0540.0440.0250.0120.0120.0120.0120.0120.0120.0120.0120.0120.0180.0210.021<0.0080.0080.0080.0080.0080.0090.090.1990.2050.1620.1350.0970*07142128formulation:150 OD* before the last treatment** Residues of each analyte calculated as spirotetramat (BYI 08330)CH Canopy height- 269 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Annex I f: Summary of trial information – CherryApplication rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksNorthern EuropeRA-2119/04R 2004 0718/1F-36300Pouligny SaintPierre, NFrancesweetcherry /Garnet1. 19932. 05.04.20043. 14.06. –18.06.20040.1440.144100010000.0140.01411.05.200425.05.2004BBCH 75 fruitfruitfruitfruitfruit0.090.430.020.010.010.150.250.320.320.230.180.210.190.110.0890.0240.0260.0810.120.130.0080.0080.0180.0230.0260.4520.9240.6290.5830.4850*0142128formulation:100 ODRA-2119/04R 2004 0720/3D-04808WurzenRoitzsch,Germanysourcherry /Fanal1. 10.03.19882. 05.05.20043. 01.08. –20.08.20040.1800.180125012500.0140.01408.06.200422.06.2004BBCH 78 fruitfruitfruitfruitfruit0.120.560.030.010.010.200.250.250.210.120.100.100.060.0330.0240.0180.0170.0210.0210.0220.0170.0140.0130.0110.0130.4550.9410.3740.2850.1890*0142128formulation:100 ODRA-2119/04R 2004 0721/1F-49800 Brainsur L’Authion,N-Francesweetcherry /Hedelfingen1. 19982. 26.04.20043. 01,07. –30,07.20040.1440.144100010000.0140.01404.06.200418.06.2004BBCH 81 fruitfruitfruitfruitfruitfruit0.030.390.030.030.020.010.700.630.790.860.580.390.110.0980.0870.110.0720.0550.0690.0570.0930.170.170.110.0540.0470.0570.110.0970.0650.9631.2221.0571.2800.9390.6300*07132127formulation:100 ODRA-2119/04R 2004 0723/8D-51399Burscheid,Germanysourcherry /Schattenmorelle1. 01.03.19992. 30.04.20043. 01.07. –20.08.20040.1440.144100010000.0140.01422.06.200406.07.2004BBCH 75 fruitfruitfruitfruitfruitfruit0.010.510.020.010.01<0.010.0990.170.410.290.210.130.0130.0140.0180.0160.0120.0120.0120.0120.0190.0300.0400.0410.0080.0080.0110.0160.0230.0200.1420.7140.4780.3620.2950.2130*07142128formulation:100 ODRA-2008/05R 2005 0068/8D-04808WurzenRoitzsch,Germanysweetcherry /Kordia1. 01.03.19962. 12.04.20053. 05.07. –20.07.20050.2160.216150015000.0140.01414.06.200528.06.2005BBCH 81 fruitfruitfruit0.690.030.020.260.530.360.0520.130.130.0740.170.230.0180.0570.0861.0940.9170.82601421formulation:150 OD- 270 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2008/05R 2005 0071/8F-36300Pouligny SaintPierre, NFrancesweetcherry /Garnet1. 01.01.19922. 01.04.20053. 16.06. –17.06.20050.1440.144100010000.0140.01412.05.200526.05.2005BBCH 75 fruitfruitfruitfruitfruitfruit0.030.280.040.020.010.010.0920.270.440.310.230.190.0720.0900.120.0820.0680.0670.0120.0120.0490.0590.0910.210.0080.0080.0110.0130.0180.0470.2140.6600.6600.4840.4170.5240*07142128formulation:150 ODRA-2008/05R 2005 0072/6D-40789Monheim,Germanysourcherry /Schattenmorelle1. 01.01.19922. 12.04.20053. 05.07. –20.07.20050.2160.216150015000.0140.01401.06.200515.06.2005BBCH 75 fruitfruitfruitfruitfruitfruit0.020.310.100.02<0.01<0.010.0410.130.300.290.150.0930.0350.0300.0460.0400.0220.0150.0120.0120.0330.0540.0370.0380.0080.0080.0240.0390.0290.0280.1160.490.5030.4430.2480.1840*07142128formulation:150 ODSouthern EuropeRA-2118/04R 2004 0716/5I-70052Bisceglie, Italysweetcherry /Lapins 011. 19942. 05.04.20043. 02.06. –22.06.20040.1440.144100010000.0140.01428.04.200412.05.2004BBCH 75 fruitfruitfruitfruitfruit0.040.250.040.01<0.010.180.220.480.380.240.220.230.190.110.0850.0290.0270.0670.110.100.0080.0080.0180.0190.0190.4770.7350.7950.6290.4540*0142128formulation:100 ODRA-2118/04R 2004 0717/3F-84170Monteux, SFrancesweetcherry /Belge1. 01.10.19992. 01.04.20043. 08.06. –22.06.20040.15840.1620110011250.0140.01411.05.200425.05.2004BBCH 78 fruitfruitfruitfruitfruitfruit0.050.430.070.060.050.020.180.280.520.500.500.350.120.120.140.110.110.0860.0240.0220.110.210.320.370.0080.0080.0210.0380.0650.0710.3820.860.8610.9181.0450.8970*09142128formulation:100 ODRA-2009/05R 2005 0073/4I-70031Andria, Italysweetcherry /Ferrovia1. 11.02.19972. 15.04.20053. 10.06. –10.07.20050.2160.216150015000.0140.01423.05.200506.06.2005BBCH 85 fruitfruitfruitfruit0.290.020.010.010.770.570.350.260.0930.0990.0550.0440.540.390.220.140.110.0730.0440.0271.8031.1520.6790.4810142128formulation:150 OD- 271 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2009/05R 2005 0074/2E-08690Santa Colomade Cervelló,Spainsweetcherry /Venus1. 15.01.19902. 05.04.20053. 15.06. –20.06.20050.19440.1944135013500.0140.01410.05.200524.05.2005BBCH 85 fruitfruitfruitfruitfruitfruit0.010.340.120.090.060.050.290.410.470.320.220.100.0720.0720.0760.0750.0730.0760.0830.0920.200.300.290.330.0170.0190.0420.0690.0780.0950.4720.9330.9080.8540.7210.6510*07142128formulation:150 OD* before the last treatment** Residues of each analyte calculated as spirotetramat (BYI 08330)- 272 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Annex I g: Summary of trial information – GrapesApplication rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksSouthern EuropeRA-2049/04R 2004 0196/5I-40128Bologna, Italygrape /Chardonnay1. 11.02.19912. 01.06.20043. 10.08. –20.08.20040.0960.096150015000.00640.006423.07.200406.08.2004BBCH 85 bunchbunchbunchbunchberrybunchberrybunchberry0.030.370.140.150.140.170.120.120.080.0400.100.110.170.150.0950.0920.0590.0410.0600.0780.0470.0950.0850.100.0720.0740.0600.0120.0120.0120.0120.0120.0120.0120.0120.0120.0410.0420.0310.110.100.160.180.160.160.1830.6020.3400.5370.4870.5370.4760.4250.3530*037714142121formulation:100 ODRA-2049/04R 2004 0197/3I-41030 SanProspero, Italygrape /Lambruscodi Sorbara1. 10.01.19962. 28.05.20043. 15.09. –10.10.20040.0960.096150015000.00640.006423.08.200406.09.2004BBCH 83 bunchbunchbunchberrybunchberrybunchberry0.140.200.200.170.030.060.030.030.0300.0420.0450.0370.0220.0350.0220.0220.0250.0270.0450.0310.0200.0380.0240.020<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0200.0180.0260.0260.0190.0380.0300.0300.2270.2990.3280.2760.1030.1830.1180.1140*07714142121formulation:100 ODRA-2049/04R 2004 0198/1GR-20006Korinthos,Greecetablegrape /Soultanina1. 10.03.19932. 15.05.20043. 20.08. –10.09.20040.0960.096150015000.00640.006410.08.200424.08.2004BBCH 85 bunchberrybunchberrybunchberrybunchberrybunchberrybunchberry0.050.050.170.140.150.120.150.160.080.080.100.080.0640.0660.0920.0890.0960.0810.110.110.110.110.110.110.0120.0120.0150.0120.0150.0130.0180.0180.0120.0130.0160.014<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0220.0230.0230.0250.0270.0250.0330.0370.0430.0450.0540.0510.160.1630.3120.2780.3000.2510.3230.3370.2570.2600.2920.2670*0*00337714142121formulation:100 OD- 273 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2049/04R 2004 0201/5E-30550Cieza, Spaintablegrape /Napoleon1. 01.01.19922. 15.04.20043. 15.09. –10.12.20040.0960.096150015000.00640.006414.09.200428.09.2004BBCH 85 bunchberrybunchberrybunchberrybunchberrybunchberrybunchberry0.220.220.320.520.450.490.370.300.200.470.210.330.0300.0310.0350.0500.0440.0400.0390.0270.0210.0470.0180.0310.0330.0320.0220.0340.0490.0500.0400.0250.0240.0540.0210.035<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0280.0280.0170.0270.0330.0310.0290.0220.0270.0580.0300.0540.3230.3230.4060.6430.5880.6230.4900.3860.2840.6410.2910.4620*0*00337715152121formulation:100 ODRA-2049/04R 2004 0202/3F-31340Vacquiers, SFrancetablegrape /Chasselas1. 01.01.19502. 01.06.20043. 15.09. –30.09.20040.0960.096150015000.00640.006419.08.200402.09.2004BBCH 85 bunchberrybunchberrybunchberrybunchberrybunchberry0.070.060.190.180.100.090.110.130.090.090.0330.0300.0410.0340.0370.0320.0440.0550.0400.0380.0120.0120.0120.0120.0120.0120.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.012<0.012<0.0120.0230.0200.0240.0240.0320.0330.0630.0740.0620.0630.150.1340.2790.2620.1930.1790.2410.2830.2160.2150*0*007714142121formulation:100 ODRA-2049/04R 2004 0203/1GR-57011Anchialos,Greecetablegrape /Moschato1. 10.02.19952. 05.06.20043. 20.08. –20.09.20040.0960.096150015000.00640.006409.08.200423.08.2004BBCH 85 bunchberrybunchberrybunchberrybunchberrybunchberry0.030.100.140.090.150.110.050.150.050.020.0240.0430.0230.0430.0570.0450.0420.0220.0340.0220.0120.0200.0120.0170.0180.0140.0120.0120.0130.012<0.0120.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0280.0930.0270.0820.0600.0360.0400.0220.0430.0310.1060.2680.2140.2440.2970.2170.1560.2180.1520.0970*0*007714142121formulation:100 OD- 274 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2034/05R 2005 0157/9E-46340Campo Arcis,Spaingrape /Tempranillo1. 01.01.19992. 15.06.20053. 15.09. –30.09.20050.0960.0968008000.01200.012030.08.200513.09.2005BBCH 85 bunchbunchbunchbunchberrybunchberrybunchberry0.090.390.320.090.110.090.070.070.060.0290.0380.0300.0300.0340.0270.0310.0220.0240.013<0.0120.0140.0170.0140.0190.0190.0180.019<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0150.0110.0130.0170.0220.0310.0350.0290.0300.1590.4630.3890.1660.1920.1790.1670.1510.1450*037714142121formulation:150 ODRA-2034/05R 2005 0157/9I-40128Bologna, Italygrape /Chardonnay1. 01.02.19952. 15.05.20053. 01.08. –10.08.20050.0960.096100010000.00960.009612.07.200526.07.2005BBCH 79 bunchbunchbunchbunchberrybunchberrybunchberry0.140.340.190.110.190.130.160.050.030.0620.0570.120.220.200.170.210.140.120.0270.0220.0260.0280.0400.0350.0410.0340.029<0.012<0.012<0.0120.0140.016<0.012<0.0120.014<0.0120.0400.0360.0390.0820.110.130.150.150.150.2810.4670.3870.4540.5560.4770.5730.3880.3410*037714142121formulation:150 ODRA-2036/05R 2005 0161/7F-86380Vendeuvre duPoitou, SFrancegrape /Chenin1. 01.03.19792. 01.06.20053. 05.10. –15.10.20050.0960.0961601600.06000.060007.09.200521.09.2005BBCH 85 bunchbunchberrybunchberrybunchberry0.210.200.140.170.160.140.12<0.0120.012<0.0120.015<0.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.0080.0090.0110.0080.0150.0170.2540.2440.1850.220.2040.1910.17307714142121formulation:048 SCRA-2036/05R 2005 0162/5I-40128Bologna, Italygrape /Chardonnay1. 01.02.19952. 15.05.20053. 01.08. –10.08.20050.0960.096100010000.00960.009613.07.200527.07.2005BBCH 79 bunchbunchberrybunchberrybunchberry0.110.080.080.100.070.030.030.0270.130.140.140.150.0990.10<0.0120.0190.0150.0260.0210.0180.018<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0140.0520.0630.0840.0950.110.110.1750.2930.310.3620.3480.2690.27007714142121formulation:048 SC* before the last treatment** Residues of each analyte calculated as spirotetramat (BYI 08330)- 275 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Annex I h: Summary of trial information – StrawberryApplication rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksGreenhouse trialsRA-2122/04R 2004 0726/2D-46397Bocholt,Germanystrawberry/ Elsanta1. 01.08.20032. 20.03.20043. 01.05. –01.06.20040.0960.096100010000.00960.009621.04.200405.05.2004BBCH 81 fruitfruitfruitfruitfruitfruit0.010.040.030.010.010.010.130.160.190.190.240.180.0120.0140.0130.0120.0120.015<0.012<0.012<0.012<0.012<0.012<0.0120.0080.0080.0080.0080.0080.0110.1720.2340.2530.2320.2820.2280*013714formulation:100 ODRA-2122/04R 2004 0765/3D-46397Bocholt,Germanystrawberry/ Dar.Selekt1. 01.08.20032. 20.03.20043. 01.05. –01.06.20040.0960.096100010000.00960.009605.05.200419.05.2004BBCH 85 fruitfruitfruitfruitfruitfruit0.010.040.010.010.010.010.160.220.130.160.150.14<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0120.0180.0220.0140.0110.0100.0190.2120.3060.1780.2050.1940.1930*013714formulation:100 ODRA-2122/04R 2004 0766/1D-53332BornheimSechtem,Germanystrawberry/ Nenci1. 26.07.20032. 10.04.20043. 12.05. –10.06.20040.1020.0966687000.01370.015326.04.200410.05.2004BBCH 85 fruitfruitfruitfruitfruitfruit0.010.080.060.040.030.020.0620.110.150.160.160.0710.0120.0130.0140.0140.0160.014<0.012<0.012<0.012<0.0120.0120.0120.0080.0090.0090.0130.0260.0300.1040.2240.2450.2390.2440.1470*013714formulation:100 ODRA-2122/04R 2004 0768/8F-82370Reynies,Francestrawberry/Gariguette1. 25.06.20032. 20.02.20043. 15.04.20040.0960.096100010000.00960.009630.03.200413.04.2004BBCH 85 fruitfruitfruitfruitfruitfruit0.010.040.020.020.010.010.120.140.140.220.280.270.0120.0120.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.0120.0120.0080.0080.0080.0130.0140.0210.1620.2120.1920.2770.3280.3250*013714formulation:100 ODRA-2122/04R 2004 0769/6D-48291TelgteWestbevern,Germanystrawberry/ Elsanta1. 01.08.20032. 20.03.20043. 01.05. –01.06.20040.0960.096100010000.00960.009621.04.200405.05.2004BBCH 85 fruitfruitfruitfruitfruit0.030.120.040.030.050.110.160.160.110.210.0120.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.0120.0080.0080.0080.0080.0080.1720.3120.2320.1720.2920*0137formulation:100 OD- 276 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2122/04R 2004 0771/8D-48291TelgteWestbevern,Germanystrawberry/ Dar.Selekt1. 01.08.20032. 20.03.20043. 01.05. –01.06.20040.0960.096100010000.00960.009621.04.200405.05.2004BBCH 85 fruitfruitfruitfruitfruit0.020.110.060.040.030.0750.140.180.160.130.0120.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.0120.0080.0090.0090.0100.0090.1270.2830.2730.2340.1930*0137formulation:100 ODRA-2122/04R 2004 0772/6D-VechtaLangförden,Germanystrawberry/ Elsanta1. 22.01.20042. 22.03.20043. 10.05. –09.06.20040.0960.0966006000.01600.016030.04.200414.05.2004BBCH 85 fruitfruitfruitfruitfruit0.040.130.110.080.080.150.180.210.170.140.0120.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.0120.0080.0080.0080.0080.0080.2220.3420.3520.2820.2520*0137formulation:100 ODRA-2122/04R 2004 0773/4F-84200Carpentras,Francestrawberry/ Pajaro1. 05.08.20032. 15.03.20043. 15.04. –15.06.20040.0960.0966006000.01600.016020.04.200404.05.2004BBCH 85 fruitfruitfruitfruitfruit0.010.030.020.020.020.180.220.230.250.210.0120.0130.0130.0130.0130.0120.0120.0120.0120.0120.0080.0080.0080.0080.0090.2220.2830.2830.3030.2640*0137formulation:100 ODField conditions – Northern EuropeRA-2120/04R 2004 0724/6D-46397Bocholt,Germanystrawberry/ Titania1. 01.08.20032. 25.04.20043. 28.05. –20.07.20040.0960.096100010000.00960.009601.06.200415.06.2004BBCH 87 fruitfruitfruitfruitfruitfruit0.010.010.010.010.01<0.010.140.0640.0840.120.140.0600.0120.0120.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.0120.0080.0080.0080.0080.0080.0080.1820.1060.1260.1620.1820.1020*013714formulation:100 ODRA-2120/04R 2004 0759/9D-48291TelgteWestbevern,Germanystrawberry/ Dar.Selekt1. 10.07.20032. 15.05. –10.06.20043. NA0.0960.096100010000.00960.009601.06.200415.06.2004BBCH 87 fruitfruitfruitfruitfruitfruit<0.010.020.010.010.01<0.010.0390.0330.0500.0880.120.0490.0120.0120.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.0120.0080.0080.0080.0080.0080.0080.0810.0850.0920.1300.1620.0910*013714formulation:100 ODRA-2120/04R 2004 0760/2F-80700Cremery, NFrancestrawberry/ Eros1. 15.01.20042. 25.05.20043. 02.06. –07.07.20040.0960.0966006000.01600.016025.05.200408.06.2004BBCH 85 fruitfruitfruitfruitfruitfruit0.010.050.020.020.010.010.0830.110.160.200.190.140.0120.0120.0120.0120.0140.019<0.012<0.012<0.012<0.012<0.0120.0120.0130.0140.0160.0140.0250.0330.1300.1980.2200.2580.2510.2140*013714formulation:100 OD- 277 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2120/04R 2004 0761/0F-80700Glisolles, NFrancestrawberry/ Mara desBois1. 18.03.20022. 10.05.20043. 26.06. –05.07.20040.0960.0966006000.01600.016014.06.200428.06.2004BBCH 87 fruitfruitfruitfruitfruitfruit<0.010.140.080.070.020.01<0.0120.0860.0780.110.120.060<0.012<0.012<0.0120.0120.0120.013<0.012<0.012<0.012<0.012<0.012<0.012<0.0080.0080.0080.0080.0090.0120.0540.2580.190.2120.1730.1070*013714formulation:100 ODField conditions – Southern EuropeRA-2121/04R 2004 0725/4I-44046 SanMartino, Italystrawberry/Marmolada1. 10.08.20032. 15.04.20043. 10.05. –30.05.20040.0960.0966006000.01600.016003.05.200417.05.2004BBCH 85 fruitfruitfruitfruitfruitfruit<0.010.040.020.020.01<0.01<0.0120.0200.0500.0800.0750.029<0.012<0.0120.0120.0120.0120.012<0.012<0.012<0.012<0.0120.012<0.012<0.008<0.0080.0080.0120.0340.0200.0540.0920.1020.1360.1430.0830*013714formulation:100 ODRA-2121/04R 2004 0762/9I-40026 Imola,Italystrawberry/Madelaine1. 01.08.20032. 05.04.20043. 10.05. –30.05.20040.0960.0966006000.01600.016026.04.200410.05.2004BBCH 81 fruitfruitfruitfruitfruitfruit<0.010.050.020.01<0.010.010.0370.0700.0800.110.0660.0420.0120.0150.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0080.008<0.0080.0080.0080.0140.0790.1550.1320.1520.1080.090*013714formulation:100 ODRA-2121/04R 2004 0763/7E-08396 SantCebrià deVallalta, Spainstrawberry/Aromas1. 05.04.20042. 05.06.20043. 30.06. –15.12.20040.0960.0968008000.01200.012006.07.200420.07.2004BBCH 87 fruitfruitfruitfruitfruit0.010.030.030.020.010.0210.0600.0890.0900.0690.0120.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.0120.0080.0080.0080.0080.0090.0630.1220.1510.1430.1140*0137formulation:100 ODRA-2121/04R 2004 0764/5F-69690Courzieu, SFrancestrawberry/ Mara desBois1. 13.04.20042. 01.07.20043. 01.08. –25.10.20040.0960.0967007000.01370.013727.09.200411.10.2004BBCH 89 fruitfruitfruitfruitfruitfruit0.010.100.060.020.010.020.0520.0580.0490.0610.0190.0120.0120.0150.0150.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.0120.0110.0110.0120.0080.0080.0080.0970.1970.1440.1130.0610.0540*013715formulation:100 OD* Before the last treatment** Residues of each analyte calculated as spirotetramat (BYI 08330)NA not applicable* before the last treatment- 278 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Annex I i: Summary of trial information – OnionApplication rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksField conditions – Northern EuropeRA-2131/04R 2004 0854/4D-40764Langenfeld,GermanyOnionStuttgarterRiesen1. 29.03.20043. 15.08.2004- 15.09.20040.0720.0720.0720.0726006006006000.01200.01200.01200.012014.07.200421.07.200428.07.200404.08.2004BBCH 48 bulbbulbbulbbulb0.04<0.01<0.01<0.010.160.160.0510.060<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.0080.2320.2020.0930.102071421formulation:100 ODRA-2131/04R 2004 0855/2F-80700Champien,FranceOnionBugati1. 01.04.20043. 28.09.2004- 30.09.20040.07200.07200.07200.07204004004004000.01800.01800.01800.018018.08.200425.08.200401.09.200408.09.2004BBCH 48 bulbbulbbulbbulb0.03<0.01<0.01<0.010.0610.0550.0450.052<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.0080.1230.0970.0870.094071421formulation:100 ODRA-2131/04R 2004 0856/0D-41379Brüggen,GermanyOnionCopra F11. 05.03.20043. 20.08.2004- 31.08.20040.07200.07200.07200.07205005005005000.01440.01440.01440.014415.07.200422.07.200429.07.200405.08.2004BBCH 48 bulbbulbbulbbulbbulbbulb0.010.040.02<0.01<0.01<0.010.0610.0630.0660.0550.0660.067<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0080.1030.1350.1180.0970.1080.10900471421formulation:100 ODRA-2131/04R 2004 0857/9F-78680Epone,FranceOnionNirvana1. 11.02.20043. 02.09.20040.07200.07200.07200.07204004004004000.01800.01800.01800.018023.07.200430.07.200406.08.200413.08.2004BBCH 47 bulbbulbbulbbulbbulbbulb<0.010.01<0.01<0.01<0.01<0.010.0470.0520.0520.0710.0580.052<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0080.0890.0940.0940.1130.1000.09400371421formulation:100 ODRA-2040/05R 2005 0212/5GB-ip24 3tqthetford,UnitedKingdomOnionRedBarron1. 14.03.20053. 15.08.2005- 31.08.20050.07200.07200.07200.07203003003003000.02400.02400.02400.024025.07.200502.08.200508.08.200515.08.2005BBCH 47 bulbbulb0.01<0.010.110.12<0.012<0.012<0.012<0.012<0.008<0.0080.1520.16208formulation:150 OD- 279 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2040/05R 2005 0214/1F-80700Champien,FranceOnionBOSTON1. 26.03.20053. 23.09.2005- 29.09.20050.07200.07200.07200.07203003003003000.02400.02400.02400.024029.08.200505.09.200512.09.200519.09.2005BBCH 49 bulbbulb0.020.01<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.0080.064<0.05407formulation:150 ODRA-2040/05R 2005 0216/8D-40764LangenfeldReusrath,GermanyOnionStuttgarterRiesen1. 26.03.20053. 16.08.20050.07200.07200.07200.07203003003003000.02400.02400.02400.024019.07.200526.07.200502.08.200509.08.2005BBCH 48 bulbbulbbulbbulbbulbbulb<0.010.01<0.01<0.01<0.01<0.010.0420.0430.0420.0420.0410.038<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0080.0840.0850.0840.0840.0830.08000371421formulation:150 ODRA-2040/05R 2005 0217/6D-53332Bornheim,GermanyOnionSumit1. 20.04.20053. 21.08.2005- 25.08.20050.07200.07200.07200.07204004004004000.01800.01800.01800.018011.07.200518.07.200525.07.200501.08.2005BBCH 47 bulbbulbbulbbulbbulbbulb<0.010.040.01<0.01<0.01<0.010.0200.0380.0400.0500.0400.031<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0080.0620.1100.0820.0920.0820.07300371521formulation:150 ODField conditions – Southern EuropeRA-2132/04R 2004 0858/7F-69380Chazayd'Azergues,FranceOnionStuttgart1. 15.04.20043. 12.08.2004- 02.09.20040.07200.07200.07200.07205005005005000.01440.01440.01440.014422.07.200429.07.200405.08.200412.08.2004BBCH 48 bulbbulbbulbbulb<0.01<0.01<0.01<0.010.0400.0210.0240.022<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.0080.0820.0630.0660.064071421formulation:100 ODRA-2132/04R 2004 0859/5GR-32200Thiva,GreeceOnionAmposta1. 20.03.20043. 05.08.2004- 08.08.20040.07200.07200.07200.07206006006006000.01200.01200.01200.012030.06.200407.07.200414.07.200421.07.2004BBCH 48 bulbbulbbulbbulb<0.01<0.01<0.01<0.010.0640.0810.0610.055<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.0080.1060.1230.1030.097071421formulation:100 ODRA-2132/04R 2004 0860/9I-40128Bologna,ItalyOnionDensity1. 22.04.20043. 10.08.2004- 25.08.20040.07200.07200.07200.07204004004004000.01800.01800.01800.018016.07.200423.07.200430.07.200406.08.2004BBCH 47 bulbbulbbulbbulbbulbbulb0.020.02<0.01<0.01<0.01<0.010.0420.0380.0500.0520.0520.056<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0080.0940.0900.0920.0940.0940.09800371421formulation:100 OD- 280 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2132/04R 2004 0861/7E-46230Alginet,SpainOnionBabosa1. 26.01.20043. 25.05.2004- 25.06.20040.07200.07200.07200.07205005005005000.01440.01440.01440.014427.04.200404.05.200412.05.200418.05.2004BBCH 47 bulbbulbbulbbulbbulbbulb<0.010.01<0.01<0.01<0.01<0.010.0900.0830.110.130.120.11<0.012<0.012<0.0120.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0080.1320.1250.1520.1720.1620.15200371421formulation:100 ODRA-2041/05R 2005 0225/7I-44012Settepolesini,ItalyOnionDorata diParma1. 27.02.20053. 20.07.2005- 15.08.20050.07200.07200.07200.07206006006006000.01200.01200.01200.012004.07.200511.07.200518.07.200525.07.2005BBCH 48 bulbbulb<0.01<0.010.0300.034<0.012<0.012<0.012<0.012<0.008<0.0080.0720.07607formulation:150 ODRA-2041/05R 2005 0226/5E-08380Malgrat deMar,SpainOnionAlabaster1. 01.08.20053. 14.11.2005- 30.11.20050.07200.07200.07770.07205005006466000.01440.01440.01200.012024.10.200502.11.200508.11.200516.11.2005BBCH 47 bulbbulb0.020.020.0320.037<0.0120.017<0.012<0.012<0.008<0.0080.0840.09407formulation:150 ODRA-2041/05R 2005 0227/3F-31790 SaintJory ,FranceOnionElody1. 13.07.20053. 24.09.2005- 01.10.20050.07200.07200.07200.07206006006006000.01200.01200.01200.012024.08.200531.08.200506.09.200513.09.2005BBCH 45 bulbbulbbulbbulbbulbbulb<0.010.010.01<0.01<0.01<0.010.0370.0510.140.100.0500.034<0.0120.015<0.0120.013<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0080.0790.0960.1820.1430.0920.07600371421formulation:150 ODRA-2041/05R 2005 0228/1E-46230Alginet,SpainOnionLiria1. 18.03.20053. 01.06.2005- 01.08.20050.07200.07200.07200.07205005005005000.01440.01440.01440.014414.06.200521.06.200528.06.200505.07.2005BBCH 48 bulbbulbbulbbulbbulbbulb<0.01<0.01<0.01<0.01<0.01<0.01<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.054<0.054<0.054<0.054<0.054<0.05400371421formulation:150 OD* Before the last treatment** Residues of each analyte calculated as spirotetramat (BYI 08330)NA not applicable- 281 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Annex I j: Summary of trial information – tomatoApplication rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksGreenhouse trialsRA-2139/04R 2004 0823/4I-70054Giovinazzo,Italycherrytomato,Shiren1. 02.08.20042. 25.08.20043. 20.10.2004- 10.12.20040.14400.14400.14400.144016001600160016000.00900.00900.00900.009012.10.200419.10.200426.10.200402.11.2004BBCH 83 fruitfruitfruitfruitfruitfruit0.120.250.110.090.110.050.200.210.190.180.170.160.0650.0560.0400.0390.0500.032<0.012<0.012<0.012<0.012<0.012<0.0120.0800.0840.0820.0960.100.110.4770.6120.4340.4170.4420.3640*01348formulation100 ODRA-2139/04R 2004 0824/2I-70056Molfetta (Bari),Italycherrytomato,Shiren1. 10.07.20042. 01.08.20043. 27.09.2004- 10.12.20040.14400.14400.14400.144016001600160016000.00900.00900.00900.009022.09.200429.09.200406.10.200413.10.2004BBCH 85 fruitfruitfruitfruitfruitfruit0.120.190.100.040.160.140.160.140.170.170.160.150.0190.0190.0140.0120.0220.020<0.012<0.012<0.012<0.012<0.012<0.0120.0650.0590.0620.0610.0820.0940.3760.4200.3580.2950.4360.4160*01348formulation100 ODRA-2139/04R 2004 0825/0E-18127JayenaGranada,Spaincherrytomato,Josefina1. 15.05.20042. 02.06.20043. 01.07.2004- 30.10.20040.15840.14400.16560.144017601600184016000.00900.00900.00900.009020.07.200427.07.200403.08.200409.08.2004BBCH 82 fruitfruitfruitfruitfruitfruit0.180.390.240.220.250.250.220.270.230.250.240.210.0130.0170.0160.0220.0210.024<0.012<0.012<0.012<0.012<0.012<0.0120.150.170.150.170.180.240.5750.8590.6480.6740.7030.7360*01357formulation100 OD3rd appl.15%overdosedRA-2139/04R 2004 0826/9E-18127FornesGranada,Spaincherrytomato,Josefina1. 13.05.20042. 02.06.20043. 01.07.2004- 30.10.20040.15840.14400.14400.144017601600160016000.00900.00900.00900.009020.07.200427.07.200403.08.200409.08.2004BBCH 82 fruitfruitfruitfruitfruitfruit0.230.270.220.250.160.160.220.210.200.230.230.210.0440.0370.0330.0450.0360.034<0.012<0.012<0.012<0.012<0.012<0.0120.120.110.120.140.140.190.6260.6390.5850.6770.5780.6060*01357formulation100 ODRA-2140/04R 2004 0827/7GR-57006Vasilica,GreeceTomatoBeatrice1. 03.08.20042. 09.08.20043. 26.10.2004- 30.11.20040.10800.10800.11660.118811251125121512380.00960.00960.00960.009628.09.200405.10.200412.10.200419.10.2004BBCH 81 fruitfruitfruitfruitfruitfruit0.040.050.040.060.030.030.110.110.190.390.230.180.0120.0120.0120.0210.0120.012<0.012<0.012<0.012<0.012<0.012<0.0120.0260.0190.0210.0310.0280.0300.2000.2030.2750.5140.3120.2640*01358formulation100 OD- 282 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2140/04R 2004 0828/5E-41720 LosPalaciosSevilla, SpainTomatoGenaro1. 20.12.20032. 05.01.20043. 01.04.2004- 30.06.20040.11520.11520.11520.115216001600160016000.00720.00720.00720.007205.05.200412.05.200418.05.200425.05.2004BBCH 85 fruitfruitfruitfruitfruitfruit0.090.100.100.090.040.090.0770.0780.0930.100.0810.0990.0120.0120.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.0120.0390.0400.0420.0430.0480.0780.2300.2420.2590.2570.1930.2910*01367formulation100 ODRA-2140/04R 2004 0829/3E-08014Viladecans,SpainTomatoMonica1. 06.02.20042. 10.03.20043. 01.04.2004- 20.07.20040.14400.13400.14400.144015001395150015000.00960.00960.00960.009614.06.200421.06.200428.06.200405.07.2004BBCH 87 fruitfruitfruitfruitfruitfruit0.110.130.140.150.150.140.0930.0730.0750.110.0790.110.0120.0120.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.0120.0340.0340.0340.0520.0390.0620.2610.2610.2730.3360.2920.3360*01347formulation100 ODRA-2140/04R 2004 0830/7I-97019Vittoria (RG),ItalyTomatoVorian1. 16.04.20042. 18.05.20043. 08.07.20040.10440.11520.12600.144014501200131315000.00720.00960.00960.009609.06.200416.06.200423.06.200430.06.2004BBCH 72 fruitfruitfruitfruitfruitfruit0.030.060.060.070.030.030.0700.0730.0790.0930.0840.0950.0120.0120.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.0120.0200.0210.0210.0280.0350.0400.1440.1780.1840.2150.1730.1890*01357formulation100 ODField conditions – Southern EuropeRA-2130/04R 2004 0849/8E-08901L'Hospitaletde Llobregat,SpainTomatoSirena1. 25.05.20042. 20.06.20043. 10.08.2004- 20.09.20040.07200.07200.07200.07207507507507500.00960.00960.00960.009627.07.200405.08.200411.08.200417.08.2004BBCH 81 fruitfruitfruitfruitfruit0.040.020.040.030.010.0450.0580.0880.0920.0750.012<0.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.0120.0180.0230.0360.0410.0410.1270.1250.1880.1870.150036713formulation100 ODRA-2130/04R 2004 0850/1P-2140-472Vale deCavalos,PortugalTomatoH-95531. 08.04.20042. 08.05.20043. 14.08.2004- 15.08.20040.07200.07200.07200.07207507507507500.00960.00960.00960.009629.06.200407.07.200413.07.200420.07.2004BBCH 86 fruitfruitfruitfruitfruit0.060.040.030.020.010.0560.0610.0570.0590.0480.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.0120.0180.0190.0260.0260.0300.1580.1440.1370.1290.112035714formulation100 OD- 283 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2130/04R 2004 0852/8GR-32001Petra, GreeceTomato8892 F11. 29.04.20042. 10.07.20043. 25.08.2004- 05.09.20040.07200.07200.07200.07207507507507500.00960.00960.00960.009626.07.200402.08.200409.08.200417.08.2004BBCH 84 fruitfruitfruitfruitfruitfruitfruit0.010.050.040.020.020.020.010.0350.0570.0570.0380.0450.0410.0340.0120.0120.0120.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0170.0240.0240.0230.0310.0260.0380.0860.1550.1450.1050.1200.1110.1060*0135714formulation100 ODRA-2130/04R 2004 0853/6I-71030Zapponeta(Fg), ItalyTomatoPerfectpeel1. 21.05.20042. 20.06.20043. 10.08.2004- 10.09.20040.07200.07200.07200.07207507507507500.00960.00960.00960.009621.07.200428.07.200404.08.200411.08.2004BBCH 81 fruitfruitfruitfruitfruitfruitfruit0.010.030.030.030.030.040.040.130.130.120.130.110.0650.0740.0120.0120.0120.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0120.0130.0150.0250.0230.0220.0420.1760.1970.1890.2090.1870.1510.1800*0135714formulation100 OD* Before the last treatment** Residues of each analyte calculated as spirotetramat (BYI 08330)NA not applicable- 284 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Annex I k: Summary of trial information – pepperApplication rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksGreenhouse trialsRA-2026/04R 2004 0113/2NL-1704 PJHeerhugowaard,NetherlandsPepper,sweetFerrari1. 15.10.20032. 15.02.20043. 15.03.20040.12240.12960.13320.136817001800185019000.00720.00720.00720.007221.04.200428.04.200405.05.200412.05.2004BBCH 82 fruitfruitfruitfruitfruitfruit0.050.100.070.080.050.040.350.380.400.410.390.460.0210.0210.0240.0240.0220.027<0.012<0.012<0.012<0.012<0.012<0.0120.0160.0170.0180.0210.0230.0260.4490.5300.5240.5470.4970.5650*01357formulation100 ODCH: 1.6-1.9mRA-2026/04R 2004 0114/0D-42799Leichlingen,GermanyPepper,sweetMazurka1. 28.05.20042. 01.06.20043. 01.08.2004- 30.09.20040.04320.04320.05040.05764504505256000.00960.00960.00960.009612.07.200419.07.200426.07.200402.08.2004BBCH 75 fruitfruitfruitfruitfruitfruit0.060.110.090.070.070.040.390.360.390.380.400.460.0210.0210.0210.0220.0250.021<0.012<0.012<0.012<0.012<0.012<0.0120.0540.0440.0530.0480.0530.0480.5370.5470.5660.5320.5600.5810*01347formulation100 ODCH: 0.6-0.8mRA-2026/04R 2004 0115/90115-04F-13690Graveson, SFrancePepper,sweetGalileo1. 30.03.20042. 10.05.20043. 10.06.2004- 15.10.20040.05040.05400.05760.06847508008509500.00670.00680.00680.007226.05.200401.06.200407.06.200414.06.2004BBCH 69 fruitfruitfruitfruitfruitfruit0.030.070.060.050.040.040.250.290.280.310.320.290.0240.0410.0280.0270.0290.025<0.012<0.012<0.012<0.012<0.012<0.0120.0190.0220.0200.0220.0250.0250.3350.4350.4000.4210.4260.3920*01357formulation100 ODCH: 0.74-0.97 mRA-2026/04R 2004 0116/7P-2000-618Póvoa daIsenta,PortugalPepper,sweetSolero1. 15.03.20042. 01.05.20043. 08.06.20040.05040.05760.06480.07205256006757500.00960.00960.00960.009618.05.200425.05.200401.06.200408.06.2004BBCH 78 fruitfruitfruitfruitfruitfruit0.030.060.030.030.040.020.290.280.250.250.260.250.0270.0300.0260.0190.0230.019<0.012<0.012<0.012<0.012<0.012<0.0120.0130.0130.0140.0140.0160.0180.3720.3950.3320.3250.3510.3190*01367formulation100 ODCH: 0.70-1.0 mRA-2026/04R 2004 0117/5I-70056Molfetta (Bari)(Puglia), ItalyPepper,sweetSienor1. 23.02.20042. 20.04.20043. 25.06.2004- 10.08.20040.10800.10800.10800.108011251125112511250.00960.00960.00960.009611.06.200418.06.200425.06.200402.07.2004BBCH 81 fruitfruitfruitfruitfruitfruit0.080.140.080.120.080.130.230.250.250.310.310.340.0150.0170.0150.0210.0190.025<0.012<0.012<0.012<0.012<0.012<0.0120.0190.0230.0200.0270.0300.0390.3560.4420.3770.4900.4510.5460*01357formulation100 ODCH: 1.0-1.1m- 285 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2026/04R 2004 0118/3D-42799Leichlingen,GermanyPepper,sweetMaratos1. 28.05.20042. 01.06.20043. 01.08.2004- 30.09.20040.04320.04320.05040.05764504505256000.00960.00960.00960.009612.07.200419.07.200426.07.200402.08.2004BBCH 75 fruitfruitfruitfruitfruitfruit0.050.110.080.070.050.050.320.300.330.260.300.350.0180.0160.0190.0150.0190.018<0.012<0.012<0.012<0.012<0.012<0.0120.0520.0360.0400.0390.0460.0500.4520.4740.4810.3960.4270.4800*01347formulation100 ODCH: 0.6-0.8mRA-2026/04R 2004 0119/1F-84210Pernes lesFontaines, SFrancePepper,sweetVolga1. 20.03.20042. 01.05.20043. 01.06.2004- 15.10.20040.05040.05400.05760.06127007508008500.00720.00720.00720.007217.05.200424.05.200401.06.200407.06.2004BBCH 68 fruitfruitfruitfruitfruitfruit0.020.030.030.030.010.020.170.180.190.200.200.180.0140.0170.0170.0160.0170.015<0.012<0.012<0.012<0.012<0.012<0.0120.0100.0100.0100.0100.0130.0130.2260.2490.2590.2680.2520.2400*01357formulation100 ODCH: 0.69-0.87 mRA-2026/04R 2004 0120/5E-08301Mataró, SpainPepper,sweetLargoitalianoPadua1. 06.03.20042. 10.04.20043. 09.06.2004- 30.11.20040.09360.10080.10800.115213001400150016000.00720.00720.00720.007228.06.200405.07.200412.07.200419.07.2004BBCH 82 fruitfruitfruitfruitfruitfruit0.030.050.060.030.030.030.370.380.420.380.420.430.0180.0190.0200.0190.0200.020<0.012<0.012<0.012<0.012<0.012<0.0120.0520.0340.0290.0360.0270.0440.4820.4950.5410.4770.5090.5360*01347formulation100 ODCH: 1.2-1.7mRA-2134/04R 2004 0791/2F-13690Graveson, SFrancePepper,sweetGalileo1. 30.03.20042. 10.05.20043. 10.06.2004- 15.10.20040.05400.05760.06120.06847508008509500.00720.00720.00720.007226.05.200401.06.200407.06.200414.06.2004BBCH 69 fruitfruitfruitfruitfruitfruit0.030.060.060.060.050.040.280.300.310.360.320.290.0290.0280.0320.0250.0280.029<0.012<0.012<0.012<0.012<0.012<0.0120.0220.0230.0210.0260.0280.0290.3730.4230.4350.4830.4380.4000*01357formulation240 CSCH: 0.75-0.95 mRA-2134/04R 2004 0792/0D-42799Leichlingen,GermanyPepper,sweetMaratos1. 28.05.20042. 01.06.20043. 01.08.2004- 30.09.20040.04320.04320.05040.05764504505256000.00960.00960.00960.009612.07.200419.07.200426.07.200402.08.2004BBCH 75 fruitfruitfruitfruitfruitfruit0.090.180.130.120.120.120.210.230.280.260.270.370.0130.0150.0160.0160.0170.021<0.012<0.012<0.012<0.012<0.012<0.0120.0260.0270.0330.0380.0310.0510.3510.4640.4710.4460.4500.5740*01347formulation240 CSCH: 0.6-0.8m- 286 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2134/04R 2004 0793/9I-70056Molfetta (Bari),ItalyPepper,sweetSienor1. 23.02.20042. 20.04.20043. 25.06.2004- 10.08.20040.10800.10800.10800.108011251125112511250.00960.00960.00960.009611.06.200418.06.200425.06.200402.07.2004BBCH 81 fruitfruitfruitfruitfruitfruit0.080.160.120.100.060.120.100.110.110.130.130.150.0120.0120.0120.0120.0120.013<0.012<0.012<0.012<0.012<0.012<0.0120.0080.0080.0090.0090.0100.0160.2120.3020.2630.2630.2240.3110*01357formulation240 CSCH: 1.5 mRA-2134/04R 2004 0794/7P-2000-618Póvoa daIsenta,PortugalPepper,sweetSolero1. 15.03.20042. 15.04.20043. 15.05.2004- 15.07.20040.05040.05760.06480.07205256006757500.00960.00960.00960.009618.05.200425.05.200401.06.200408.06.2004BBCH 78 fruitfruitfruitfruitfruitfruit0.040.090.050.040.020.030.200.200.210.210.180.190.0130.0230.0150.0140.0120.012<0.012<0.012<0.012<0.012<0.012<0.0120.0100.0120.0110.0130.0130.0170.2750.3370.2980.2890.2370.2600*01367formulation240 CSCH: 0.7-1.0mField conditions – Southern EuropeRA-2027/04R 2004 0121/3E-46230Alginet, SpainPepper,sweetItalico1. 29.04.20042. 20.05.20043. 10.06.2004- 30.08.20040.07200.07200.07200.07206006006008000.01200.01200.01200.009016.06.200423.06.200430.06.200406.07.2004BBCH 72 fruitfruitfruitfruitfruitfruit0.130.280.200.140.080.100.510.510.550.540.510.480.0340.0390.0570.0620.0470.053<0.012<0.012<0.012<0.012<0.012<0.0120.0510.0430.0500.0630.0530.0660.7370.8840.8690.8170.7020.7110*01367formulation100 ODRA-2027/04R 2004 0122/1F-31 330 LeBurgaud,FrancePepper,sweetAlby1. 17.05.20042. 10.06.20043. 01.08.2004- 01.10.20040.07200.07200.07890.07207507508237500.00960.00960.00960.009623.07.200430.07.200406.08.200413.08.2004BBCH 76 fruitfruitfruitfruitfruitfruit<0.010.010.010.01<0.01<0.010.190.190.150.210.180.210.0120.0120.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.0120.0160.0140.0130.0190.0170.0220.240.2380.1970.2630.2310.2660*01357formulation100 OD3rdapplicationwas 10%overdosedRA-2027/04R 2004 0124/8I-70054Giovinazzo(Bari), ItalyPepper,sweetComet1. 21.06.20042. 30.07.20043. 15.09.2004- 31.10.20040.07200.07200.07200.072010001000100010000.00720.00720.00720.007207.09.200414.09.200421.09.200428.09.2004BBCH 74 fruitfruitfruitfruitfruitfruit<0.010.010.010.01<0.01<0.010.110.120.130.130.160.120.0120.0120.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.0120.0100.0090.0090.0100.0120.0110.1540.1630.1730.1740.2060.1650*01357formulation100 OD- 287 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2027/04R 2004 0125/6P-2120-193Foros deSalvaterra,PortugalPepper,sweetClaudio1. 02.05.20042. 10.06.20040.07610.07200.07200.07207937507507500.00960.00960.00960.009625.06.200402.07.200409.07.200416.07.2004BBCH 77 fruitfruitfruitfruitfruitfruit0.020.040.040.020.020.020.230.250.240.250.290.290.0120.0120.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.0120.0150.0140.0130.0150.0180.0190.2890.3280.3170.3090.3520.3530*01357formulation100 OD1stapplicationwas 6 %overdosedRA-2039/05R 2005 0200/1I-70053Canosa (Bari),ItalyPepper,sweetTopeto1. 02.06.20052. 01.07.20053. 15.08.2005- 15.09.20050.07200.07200.07200.07208008008008000.00900.00900.00900.009002.08.200509.08.200516.08.200523.08.2005BBCH 85 fruitfruitfruitfruitfruitfruit0.010.030.040.020.010.010.0580.0480.0490.0520.0670.0920.0120.0120.0120.0120.0120.013<0.012<0.012<0.012<0.012<0.012<0.0120.0080.0080.0080.0080.0100.0120.1000.1100.1210.1040.1110.1390*01357formulation150 ODRA-2039/05R 2005 0202/8P-2140-427CaniceiraVale deCavalos,PortugalPepper,sweetTorpedo1. 08.04.20052. 15.05.20053. 10.07.2005- 30.09.20050.07200.07200.07200.07205005005005000.01440.01440.01440.014413.06.200520.06.200527.06.200504.07.2005BBCH 77 fruitfruitfruitfruitfruitfruit0.010.030.010.010.010.010.130.150.130.120.130.0980.0120.0120.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.0120.0080.0080.0080.0080.0080.0080.1720.2120.1720.1620.1720.1400*01357formulation150 ODRA-2046/05R 2005 0707/0I-70053Canosa diPuglia (Bari),ItalyPepper,sweetTopeto1. 02.06.20052. 01.07.20053. 15.08.2005- 15.09.20050.07200.07200.07200.07208008008008000.00900.00900.00900.009002.08.200509.08.200516.08.200523.08.2005BBCH 85 fruitfruitfruitfruitfruitfruit0.010.040.030.020.010.010.0430.0500.0440.0530.0470.0690.0120.0120.0120.0140.0120.013<0.012<0.012<0.012<0.012<0.012<0.0120.0080.0080.0080.0080.0080.0090.0850.1220.1060.1070.0890.1130*01357formulation048 SCRA-2046/05R 2005 0708/9P-2140-427Caniceira -Vale deCavalos,PortugalPepper,sweetTorpedo1. 08.04.20052. 15.05.20053. 10.07.2005- 30.09.20050.07200.07200.07200.07205005005005000.01440.01440.01440.014413.06.200520.06.200527.06.200504.07.2005BBCH 77 fruitfruitfruitfruitfruitfruit0.010.040.020.020.020.010.0890.110.0960.120.110.110.0120.0120.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.0120.0080.0080.0080.0080.0080.0080.1310.1820.1480.1720.1620.1520*01357formulation048 SC* Before the last treatment** Residues of each analyte calculated as spirotetramat (BYI 08330)NA not applicableCH Height of leafy surface- 288 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Annex I l: Summary of trial information – cucumberApplication rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksGreenhouse trialsRA-2030/04R 2004 0130/2D-42799Leichlingen,GermanyCucumberEscape1. 04.05.20042. 15.05.20043. 15.06.2004- 15.08.20040.10080.12960.14400.144010501350150015000.00960.00960.00960.009628.05.200404.06.200411.06.200418.06.2004BBCH 75fruitfruitfruitfruitfruitfruit<0.010.020.020.02<0.01<0.01<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0170.0170.0230.013<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.0540.0690.0690.0750.055<0.0540*01357formulationOD 100CH: 1.4-2.0mRA-2030/04R 2004 0131/0I-97017 SantaCroceCamerina,ItalyCucumberSolverde1. 06.09.20042. 20.09.20043. 11.10.2004- 22.11.20040.14400.14400.14400.144015001500150015000.00960.00960.00960.009613.10.200420.10.200427.10.200403.11.2004BBCH 89fruitfruitfruitfruitfruitfruit<0.010.020.030.01<0.01<0.01<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0120.0150.0170.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.0540.0640.0770.059<0.054<0.0540*01357formulationOD 100CH: 2.0 mRA-2030/04R 2004 0132/9E-08014Viladecans,SpainCucumberFito Porto1. 05.03.20042. 01.04.20043. 25.04.2004- 19.07.20040.11520.12240.13680.144012001275142515000.00960.00960.00960.009612.05.200419.05.200426.05.200402.06.2004BBCH 85 fruitfruitfruitfruitfruitfruit<0.010.040.030.02<0.01<0.01<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0200.0200.018<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.0540.0920.0820.070<0.054<0.0540*01357formulationOD 100CH: 1.15-1.44 mRA-2030/04R 2004 0133/7GR-60100Aronas,GreeceCucumberLuberon1. 30.06.20042. 15.07.20043. 05.08.2004- 07.09.20040.03600.07200.10800.1296375750112513500.00960.00960.00960.009627.07.200403.08.200410.08.200417.08.2004BBCH 77 fruitfruitfruitfruitfruitfruit<0.010.030.050.020.020.01<0.0120.0220.016<0.012<0.012<0.012<0.0120.0220.0200.0220.0150.013<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.0540.0940.1060.0740.0670.0550*01357formulationOD 100CH: 0.5-1.8mRA-2030/04R 2004 0134/5D-42799Leichlingen,GermanyCucumberIndira1. 04.06.20042. 15.06.20043. 15.07.2004- 15.09.20040.11520.14400.14400.144012001500150015000.00960.00960.00960.009625.06.200402.07.200409.07.200416.07.2004BBCH 75 fruitfruitfruitfruitfruitfruit0.020.050.050.030.02<0.01<0.012<0.012<0.012<0.012<0.012<0.0120.0190.0240.0190.0150.020<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0080.0710.1060.1010.0770.072<0.0540*01357formulationOD 100CH: 1.6-2.0m- 289 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2030/04R 2004 0135/3I-70056Molfetta (Bari),ItalyCucumberLocale diPolignano1. 17.03.20042. 10.04.20043. 20.05.2004- 20.07.20040.14400.14400.14400.144015001500150015000.00960.00960.00960.009619.05.200426.05.200402.06.200409.06.2004BBCH 76 fruitfruitfruitfruitfruitfruit<0.010.010.01<0.01<0.01<0.01<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0260.015<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.0540.0680.057<0.054<0.054<0.0540*01357formulationOD 100CH: 2.0 mRA-2030/04R 2004 0136/1E-04740Roquetas deMar, SpainCucumberCaman1. 23.03.20042. 05.05.20043. 15.04.2004- 30.06.20040.12240.14400.14400.144012751500150015000.00960.00960.00960.009618.05.200425.05.200401.06.200408.06.2004BBCH 74 fruitfruitfruitfruitfruitfruit<0.010.02<0.01<0.01<0.01<0.01<0.0120.0190.012<0.012<0.012<0.0120.0130.0380.0390.015<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0080.0550.0970.0810.057<0.054<0.0540*01367formulationOD 100CH: 1.7-2.0mRA-2030/04R 2004 0138/8GR-58300Esovalta,GreeceCucumberScotinos(Hybrid.1. 20.07.20042. 01.08.20043. 16.08.20040.03600.07200.08640.108037575090011250.00960.00960.00960.009602.08.200409.08.200416.08.200423.08.2004BBCH 74 fruitfruitfruitfruitfruitfruit<0.010.040.01<0.01<0.01<0.01<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0480.0210.013<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.0540.1200.063<0.054<0.054<0.0540*01357formulationOD 100CH: 0.5-1.5mField conditions – Southern EuropeRA-2028/04R 2004 0126/4E-41310Brenes, SpainCucumberSuso1 15.04.20042 15.05.20043 15.05.2004- 15.07.20040.07200.07200.07200.07206006006006000.01200.01200.01200.012026.05.200402.06.200408.06.200415.06.2004BBCH 85 fruitfruitfruitfruitfruitfruit<0.010.040.020.020.010.01<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0180.015<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.0540.0900.0670.064<0.054<0.0540*01367formulationOD 100RA-2028/04R 2004 0128/0E-08380Malgrat deMar, SpainCucumberOporto1 23.06.20042 09.07.20043 02.08.2004- 30.09.20040.07200.07200.07200.0720800900100010000.00900.00800.00720.007223.07.200428.07.200403.08.200410.08.2004BBCH 82 fruitfruitfruitfruitfruitfruit<0.01<0.01<0.01<0.01<0.01<0.01<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.054<0.054<0.054<0.054<0.054<0.0540*01367formulationOD 100- 290 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2028/04R 2004 0129 9I-71030ZapponetaFoggia, ItalyCucumberMarinda1 15.07.20042 01.08.20043 20.08.2004- 20.09.20040.07200.07200.07200.07208008008008000.00900.00900.00900.009006.08.200413.08.200420.08.200427.08.2004BBCH 89 fruitfruitfruitfruitfruitfruit<0.010.020.01<0.01<0.01<0.01<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0330.0150.013<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.0540.0850.057<0.054<0.054<0.0540*01357formulationOD 100RA-2043/05R 2005 0239/7E-46230Alginet, SpainCucumberRaider1. 12.05.20052. 01.06.20053. 20.06.2005- 10.08.20050.07200.07200.07200.07206006006008000.01200.01200.01200.009014.06.200521.06.200528.06.200505.07.2005BBCH 73 fruitfruitfruitfruitfruitfruit<0.010.030.020.02<0.01<0.01<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.0540.0740.0640.064<0.054<0.0540*01367formulationOD 150RA-2043/05R 2005 0240/0E-08380Malgrat deMar, SpainCucumberKenia1. 14.05.20052. 30.05.20053. 15.06.2005- 30.08.20050.07920.07200.07200.072077080090010000.01040.00900.00800.007223.06.200501.07.200508.07.200515.07.2005BBCH 84 fruitfruitfruitfruit<0.01<0.01<0.01<0.01<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.054<0.054<0.054<0.0540357formulationOD 1501stapplication10%overdosedRA-2043/05R 2005 0241/9I-97019Vittoria, ItalyCucumberSetman1. 30.06.20052. 15.07.20053. 15.08.2005- 15.09.20050.07200.07200.07200.07206006008008000.01200.01200.00900.009027.07.200503.08.200510.08.200517.08.2005BBCH 78 fruitfruitfruitfruit0.01<0.01<0.01<0.010.017<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.0080.059<0.054<0.054<0.0540357formulationOD 150RA-2043/05R 2005 0715 1I-71049Zapponeta,ItalyCucumberLocale diPolignano1. 20.09.20052. 20.10.20053. 30.10.2005- 30.12.20050.07200.07200.07200.07207007007007000.01040.01040.01040.010427.10.200503.11.200510.11.200517.11.2005BBCH 88 fruitfruitfruitfruitfruitfruit0.030.060.070.060.050.030.0210.0350.0250.0270.0200.019<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0080.0830.1270.1270.1190.1020.0810*01357formulationOD 150* Before the last treatment** Residues of each analyte calculated as spirotetramat (BYI 08330)NA not applicableCH Height of leafy surface- 291 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Annex I m: Summary of trial information – melonApplication rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksGreenhouse trialsRA-2128/04R 2004 0836/6I-70056Molfetta, ItalyMelonIncas1 15.03.20042 20.04.20043 15.06.2004- 15.07.20040.07200.07200.07200.07208008008008000.00900.00900.00900.009001.06.200408.06.200415.06.200422.06.2004BBCH 83 fruitfruitfruitfruitpulppeelfruitpulppeelfruit0.010.020.020.01<0.010.050.02<0.010.020.02<0.012<0.012<0.012<0.012<0.0120.019<0.012<0.0120.015<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.0540.0640.064<0.054<0.0540.1010.064<0.0540.0670.0640*013335557formulation:OD 100RA-2128/04R 2004 0837/4E-11540Sanlucar deBda (MonteAlgaida),SpainMelonPrimal1 26.04.20042 20.05.20043 30.06.2004- 10.07.20040.07200.07200.07200.072010001000100010000.00720.00720.00720.007209.06.200416.06.200423.06.200429.06.2004BBCH 79 fruitfruitfruitfruitpulppeelfruitpulppeelfruit<0.010.020.02<0.01<0.010.01<0.01<0.010.02<0.01<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.021<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.015<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.0540.0640.064<0.054<0.054<0.054<0.054<0.0540.076<0.0540*013335557formulation:OD 100RA-2128/04R 2004 0838/2F-84140Montfavet, SFranceMelonLunabel1 25.03.20042 15.04.20043 15.06.2004- 05.07.20040.07200.07200.07200.07206006006006000.01200.01200.01200.012027.05.200402.06.200409.06.200416.06.2004BBCH 82 fruitfruitfruitfruitpulppeelfruitpulppeelfruit<0.01<0.01<0.010.01<0.010.02<0.01<0.010.02<0.01<0.012<0.012<0.0120.014<0.0120.027<0.012<0.0120.024<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.054<0.054<0.0540.056<0.0540.079<0.054<0.0540.076<0.0540*013336667formulation:OD 100- 292 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2128/04R 2004 0839/0P-2560-014TorresVedras,PortugalMelonGalas1 02.04.20042 25.05.20043 07.07.2004- 14.07.20040.07200.07200.07200.072010001000100010000.00720.00720.00720.007217.06.200424.06.200401.07.200408.07.2004BBCH 85 fruitfruitfruitfruitpulppeelfruitpulppeelfruit<0.010.010.010.01<0.010.040.01<0.010.030.01<0.012<0.012<0.012<0.012<0.0120.017<0.012<0.0120.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0150.012<0.0120.029<0.012<0.0120.027<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.054<0.0540.057<0.054<0.0540.106<0.054<0.0540.089<0.0540*013335557formulation:OD 100RA-2128/04R 2004 0840/40840-04P-2565Freiria,PortugalMelonStar King1 02.05.20042 25.05.20043 07.07.2004- 14.07.20040.07200.07200.07200.072010001000100010000.00720.00720.00720.007209.06.200416.06.200423.06.200430.06.2004BBCH 81 fruitfruitfruitfruitpulppeelfruitpulppeelfruit<0.01<0.01<0.01<0.01<0.01<0.010.01<0.010.020.01<0.012<0.012<0.012<0.012<0.0120.012<0.012<0.0120.020<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.054<0.054<0.054<0.054<0.054<0.054<0.054<0.0540.072<0.0540*013335557formulation:OD 100RA-2128/04R 2004 0841/2I-71043Manfredonia(Fg), ItalyMelonDrake1 07.04.20042 05.05.20043 04.07.2004- 20.07.20040.07200.07200.07200.072010001000100010000.00720.00720.00720.007215.06.200422.06.200429.06.200406.07.2004BBCH 81 fruitfruitfruitfruitpulppeelfruitpulppeelfruit<0.01<0.01<0.01<0.01<0.010.01<0.01<0.010.02<0.01<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.013<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.054<0.054<0.054<0.054<0.054<0.054<0.054<0.0540.065<0.0540*013335557formulation:OD 100- 293 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2128/04R 2004 0881/1E-41720 LosPalaciosSevilla, SpainMelonMontijo1 05.02.20042 01.04.20043 01.06.2004- 01.07.20040.07200.07200.07200.072010001000100010000.00720.00720.00720.007210.05.200417.05.200424.05.200431.05.2004BBCH 84 fruitfruitfruitfruitpulppeelfruitpulppeelfruit<0.01<0.01<0.01<0.01<0.010.01<0.01<0.010.010.010.0120.0170.0190.015<0.0120.022<0.012<0.0120.0150.019<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.0540.0590.0610.057<0.0540.064<0.054<0.0540.0570.0610*013334447formulation:OD 100RA-2128/04R 2004 0883/8F-31 340VACQUIERS,FranceMelonPorphyre1 29.03.20042 29.04.20043 18.06.2004- 30.06.20040.07200.07200.07200.072010001000100010000.00720.00720.00720.007228.05.200404.06.200411.06.200418.06.2004BBCH 82 fruitfruitfruitfruitpulppeelfruitpulppeelfruit<0.01<0.01<0.01<0.01<0.010.01<0.01<0.01<0.01<0.01<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.054<0.054<0.054<0.054<0.054<0.054<0.054<0.054<0.054<0.0540*013335557formulation:OD 100Field conditions – Southern EuropeRA-2129/04R 2004 0842/0I-70031 Andria(Bari), ItalyMelonExsalto1. 10.04.20042. 20.05.20043. 10.07.2004- 31.07.20040.07200.07200.07200.07207507507507500.00960.00960.00960.009624.06.200401.07.200408.07.200415.07.2004BBCH 88 fruitfruitfruitfruitpulppeelfruitfruitpulppeel0.020.050.050.04<0.010.080.040.03<0.010.10<0.012<0.0120.014<0.012<0.0120.021<0.012<0.012<0.0120.025<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.0080.0640.0940.0960.084<0.0540.1330.0840.074<0.0540.1570*013335777formulation:OD 100- 294 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2129/04R 2004 0843/9E-08850 Gava(Barcelona),SpainMelonBraco1. 05.05.20042. 10.06.20043. 30.07.2004- 20.08.20040.07200.07200.07200.07207007007007000.01030.01030.01030.010320.07.200426.07.200402.08.200409.08.2004BBCH 89 fruitfruitpulppeelfruitfruitpulppeel<0.01<0.01<0.010.02<0.01<0.01<0.01<0.01<0.012<0.012<0.0120.026<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.054<0.054<0.0540.078<0.054<0.054<0.054<0.05413334777formulation:OD 100RA-2129/04R 2004 0844/7E-46230Alginet, SpainMelonSancho1. 01.06.20042. 20.06.20043. 01.08.2004- 30.08.20040.07200.07200.07200.07207507507507500.00960.00960.00960.009620.07.200427.07.200403.08.200410.08.2004BBCH 89 fruitfruitfruitfruitpulppeelfruitfruitpulppeel0.020.030.020.02<0.010.060.020.01<0.010.030.0250.0430.0270.036<0.0120.0730.0260.021<0.0120.041<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.0080.0770.1050.0790.088<0.0540.1650.0780.063<0.0540.1030*013336777formulation:OD 100RA-2129/04R 2004 0845/5GR-60100Aronas,GreeceMelonSupra1. 08.06.20042. 30.06.20043. 05.08.2004- 15.10.20040.07200.07200.07200.07205005005005000.01440.01440.01440.014427.07.200403.08.200410.08.200417.08.2004BBCH 89 fruitfruitfruitfruitpulppeelfruitfruitpulppeel<0.010.010.020.01<0.010.01<0.01<0.01<0.010.01<0.0120.0190.020<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.0540.0610.072<0.054<0.054<0.054<0.054<0.054<0.054<0.0540013335777formulation:OD 100- 295 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2042/05R 2005 0230/3GR-60100AronasKaterini,GreeceMelonGallia1. 27.05.20052. 10.06.20053. 22.07.2005- 03.08.20050.07200.07200.07200.07206006006006000.01200.01200.01200.012001.07.200508.07.200515.07.200522.07.2005BBCH 86 fruitfruitpulppeelfruitpulppeelfruitpulppeel0.01<0.01<0.010.02<0.01<0.010.02<0.01<0.01<0.01<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0490.0370.0330.0320.0230.0220.0280.0310.0220.019<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.0080.0910.0790.0750.0840.0650.0640.0800.0730.0640.0610333555777formulation:OD 150RA-2042/05R 2005 0231/1E-08850 Gava(Barcelona),SpainMelonSANCHO1. 04.05.20052. 25.05.20053. 15.08.2005- 20.09.20050.07200.07200.06690.07206006005586000.01200.01200.01200.012005.08.200512.08.200519.08.200526.08.2005BBCH 89 fruitfruitpulppeelfruitpulppeelfruitpulppeel<0.01<0.01<0.010.03<0.01<0.010.02<0.01<0.010.020.0140.014<0.0120.041<0.012<0.0120.029<0.012<0.0120.015<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.0080.0560.056<0.0540.103<0.054<0.0540.081<0.054<0.0540.0670333555777formulation:OD 150RA-2042/05R 2005 0233/8P-2580-102AldeiaGavinha,PortugalMelonAlbino1. 15.05.20052. 01.06.20053. 20.07.2005- 05.08.20050.07200.07200.07200.07208008008008000.00900.00900.00900.009027.06.200504.07.200511.07.200518.07.2005BBCH 87 fruitfruitfruitpulppeelfruitpulppeelfruitpulppeelfruitpulppeel<0.01<0.01<0.01<0.01<0.01<0.01<0.01<0.01<0.01<0.01<0.01<0.01<0.01<0.01<0.0120.0160.021<0.0120.0410.017<0.0120.0360.015<0.0120.0310.012<0.0120.023<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.0540.0580.063<0.0540.0830.059<0.0540.0780.057<0.0540.073<0.054<0.0540.0650*0111333444777formulation:OD 150- 296 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2042/05R 2005 0234/6I-95040Licodia Eubea(CT.), ItalyMelonHelios1. 06.05.20052. 01.06.20053. 20.07.2005- 20.08.20050.07200.07200.07200.072060060080010000.01200.01200.00900.007208.07.200515.07.200522.07.200529.07.2005BBCH 84 fruitfruitfruitfruitpulppeelfruitpulppeelfruitpulppeel<0.010.01<0.01<0.01<0.01<0.01<0.01<0.01<0.01<0.01<0.01<0.01<0.012<0.012<0.012<0.012<0.0120.031<0.012<0.0120.016<0.012<0.0120.015<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.054<0.054<0.054<0.054<0.0540.073<0.054<0.0540.058<0.054<0.0540.0570*01333555777formulation:OD 150RA-2042/05R 2005 0717/8E-46230Alginet, SpainMelonSirio1. 12.05.20052. 10.06.20053. 01.07.2005- 10.08.20050.07200.07200.07200.07208008008008000.00900.00900.00900.009001.07.200511.07.200518.07.200525.07.2005BBCH 89 fruitfruitfruitfruitpulppeelfruitpulppeelfruitpulppeel<0.01<0.01<0.01<0.01<0.01<0.01<0.01<0.01<0.01<0.01<0.01<0.01<0.0120.013<0.012<0.012<0.0120.018<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.0540.055<0.054<0.054<0.0540.060<0.054<0.054<0.054<0.054<0.054<0.0540*01333444777formulation:OD 1501st sprayinterval 10days,because ofbadweatherconditions* Before the last treatment** Residues of each analyte calculated as spirotetramat (BYI 08330)- 297 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Annex I n: Summary of trial information – floweringbrassicaApplication rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksField trials, northern EuropeRA-2022/04R 2004 0105/1D-40764LangenfeldGermanybroccoliMarathon1. 27.04.20043. 15.07.20040.07200.07200.07203003003000.0240.0240.02415.06.200422.06.200429.06.2004BBCH 45 curdcurdcurdcurdcurd<0.010.080.070.010.010.170.170.200.140.0970.210.220.280.200.12<0.012<0.012<0.012<0.012<0.0120.0130.0130.0160.0120.0080.4150.4950.5780.3740.2470*03713formulation:100 OD;RA-2022/04R 2004 0108/6GB-NR29 5DSRollesbyUnitedKingdombroccoliMarathon1. 07.07.20042. 07.09.2004- 30.09.20043. 21.09.2004- 28.09.20040.07740.07200.07203233003000.0240.0240.02424.08.200431.08.200407.09.2004BBCH 41 curdcurdcurdcurdcurdcurd0.010.240.09<0.01<0.01<0.010.290.480.280.290.180.150.0670.140.130.130.100.048<0.012<0.012<0.012<0.012<0.012<0.0120.0090.0080.0090.0080.0080.0080.3880.8800.5210.4500.3100.2280*0371421formulation:100 ODRA-2023/04R 2004 109/4D-40764LangenfeldGermanycauliflowerFreedom1. 27.04.20042. no data3.15.07.20040.07200.07200.07203003003000.0240.0240.02415.06.200422.06.200429.06.2004BBCH42 - 43curdcurdcurdcurdcurd<0.010.02<0.01<0.01<0.010.0740.0330.0550.0190.0130.200.240.340.280.14<0.012<0.012<0.012<0.012<0.0120.0080.0110.0100.0100.0080.3040.3160.4270.3310.1830*03713formulation:100 ODRA-2023/04R 2004 0110/8F-27340Criquebeuf surSeineN-FrancecauliflowerAVISO1. 15.06.20042. no data3. 19.10.20040.07200.07200.07203003003000.0240.0240.02421.09.200428.09.200405.10.2004BBCH 48 curdcurdcurdcurdcurdcurd<0.010.010.02<0.01<0.01<0.010.0350.0790.0770.140.150.120.0340.0480.0460.0690.0610.076<0.012<0.012<0.012<0.012<0.012<0.0120.0080.0080.0080.0080.0080.0080.0990.1570.1630.2390.2410.2260*0371421formulation:100 ODRA-2062/05R 2005 0363/6D-42799LeichlingenGermanybroccoliVolta F11. 01.06.20053. 25.06.2005- 30.07.20050.0720.0720.0725005005000.0140.0140.01430.06.200514.07.200528.07.2005BBCH 45 curdcurdcurdcurdcurdcurdcurdcurd0.570.190.010.100.01<0.01<0.01<0.010.250.240.0730.260.140.180.890.0920.100.180.0740.170.130.150.0470.038<0.012<0.012<0.012<0.012<0.012<0.012<o.012<0.012<0.0080.0190.0110.0080.0210.0320.0110.0110.9400.6410.1800.5500.3130.3840.1690.163-14-110*0371421formulation:150 OD- 298 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2062/05R 2005 0364/4F-80200EnnemainN-FrancebroccoliLord1. 18.05.20052. 25.07.2005- 10.08.20050.0720.0720.0725005005000.0140.0140.01401.07.200515.07.200529.07.2005BBCH 48 curdcurdcurdcurdcurdcurd0.090.030.110.010.010.010.280.120.0780.0480.0460.0330.120.0820.0470.0320.0250.022<0.012<0.012<0.012<0.012<0.012<0.012<0.0080.0180.008<0.008<0.0080.0080.5100.2620.2550.1100.1010.085-14-1103714formulation:150 ODRA-2062/05R 2005 0365/2D-67125SchauernheimGermanycauliflowerCegano1. 25.07.20053. 13.10.2005- 10.11.20050.0720.0720.0725005005000.0140.0140.01414.09.200528.09.200512.10.2005BBCH 49 curdcurdcurdcurdcurdcurdcurdcurd0.01<0.01<0.010.020.020.020.01<0.010.110.150.0910.130.140.130.120.0860.0270.0290.0230.0480.0400.0310.0340.030<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.0080.0080.008<0.0080.0080.0080.1670.2090.1440.2180.2200.2010.1840.146-14-110*0371421formulation:150 ODRA-2062/05R 2005 1017/9D-88074MecklenbeurenGermanybroccoliIron Man1. 22.07.20053. 01.10.2005- 31.10.20050.0720.0726006000.0120.01213.09.200527.09.2005BBCH 46 curdcurd0.070.010.150.180.0990.098<0.012<0.0120.0080.0080.3390.30803formulation:150 ODRA-2062/05R 2005 1047/0GB-IP10 ORAIpswichUnitedKingdomcauliflowerAlpen1. 30.07.20053. 01.03.2006- 21.03.20060.0720.0720.0725005005000.0140.0140.01418.01.200601.02.200622.02.2006BBCH 45 curdcurdcurdcurdcurdcurd<0.01<0.01<0.01<0.01<0.01<0.010.0790.120.230.240.310.250.0120.0120.0360.0590.0290.039<0.0120.012<0.012<0.012<0.0120.012<0.008<0.008<0.008<0.008<0.008<0.0080.1210.1620.2960.3290.3690.319-21-1903713formulation:150 ODField trials, Southern EuropeRA-2024/04R 2004 0111/6I-71030ZapponetaItalybroccoliMarathon1. 05.08.20043. 20.11.2004- 30.12.20040.07200.07200.07208008008000.0090.0090.00912.11.200419.11.200426.11.2004BBCH 47 curdcurdcurdcurdcurd0.040.130.020.020.010.130.190.200.310.250.0690.0940.0800.0890.068<0.012<0.012<0.012<0.012<0.012<0.0080.008<0.0080.0080.0080.2590.4340.3200.4390.3480*03714formulation:100 OD- 299 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2025/04R 2004 0112/4F-31150FenouilletS-FrancecauliflowerFlamenco1. 02.08.20042. no data3. 30.10.2004- 30.11.20040.07200.07200.07205005005000.0140.0140.01426.10.200402.11.200409.11.2004BBCH 49 curdcurdcurdcurdcurdcurd<0.01<0.01<0.01<0.01<0.01<0.010.0750.0950.0770.130.130.110.0670.0780.0810.100.0740.067<0.012<0.012<0.012<0.012<0.012<0.0120.0080.0080.0080.0080.0080.0080.1720.2030.1880.2600.2340.2070*0371420formulation:100 ODRA-2063/05R 2005 0360/1I-71043ManfredoniaItalybroccoliMarathon1. 10.08.20053. 10.11.2005- 10.12.20050.0720.0720.0726006006000.0120.0120.01219.10.200502.11.200516.11.2005BBCH 45 curdcurdcurdcurdcurdcurdcurdcurd0.080.060.010.110.010.010.01<0.010.110.0990.110.150.110.120.130.0870.0370.0360.0250.0430.0290.0350.0360.026<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0080.0080.0080.0080.0080.0080.0080.0110.2470.2150.1650.3230.1690.1850.1960.146-14-110*0381420formulation:150 ODRA-2063/05R 2005 0362/8E-08850 GavaSpaincauliflowerFloraBlanca1. 04.02.20063. 10.05.2006- 20.05.20060.0720.0720.0726006006000.0120.0120.01211.04.200625.04.200609.05.2006BBCH 43 whole pl.whole pl.curdcurdcurdcurd1.00.060.010.130.01<0.010.230.100.0390.0850.0700.0840.0490.0190.0120.0130.0130.014<0.0120.012<0.012<0.012<0.012<0.0120.0080.0080.0080.0130.0080.0101.2990.1990.0810.2530.1130.130-14-110*037formulation:150 OD* Before the last treatment** Residues of each analyte calculated as spirotetramat (BYI 08330)whole pl. whole plant without roots- 300 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Annex I o: Summary of trial information – BrusselssproutsApplication rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksField trials, northern EuropeRA-2039/04R 2004 0160/4D-53773HennefGermanybrusselssproutsIgor F11. 06.05.20043. 01.10.2004- 31.12.20040.07200.07200.07205005005000.0140.0140.01430.09.200407.10.200414.10.2004BBCH 48 sproutsproutsproutsproutsprout0.010.030.010.010.010.0220.0440.0410.0510.0530.0120.0160.0130.0250.014<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.080.0640.110.0840.1060.0970*03714formulation:100 ODRA-2039/04R 2004 0161/2D-40764Langenfeld,GermanybrusselssproutsGenius1. 27.04.20043. 15.10.2004- 15.11.20040.07200.07200.07205005005000.0140.0140.01417.09.200424.09.200401.10.2004BBCH 47 sproutsproutsproutsproutsprout<0.010.010.010.010.010.0120.0180.0210.0350.0410.0120.0130.0120.0180.017<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0540.0610.0630.0830.0880*03714formulation:100 ODRA-2039/04R 2004 0162/0F-27340Criqubeuf surSeineN- FrancebrusselssproutsRomulus1. 16.06.20043. 15.11.20040.07200.07200.07205005005000.0140.0140.01412.10.200422.10.200425.10.2004BBCH 46 sproutsproutsproutsproutsproutsprout0.010.020.01<0.01<0.01<0.010.0230.0430.0390.0690.0510.0510.0230.0340.0250.0320.0230.016<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0080.0760.1170.0940.1310.1040.0970*0381421formulation:100 ODRA-2039/04R 2004 0163/9F-62390FontaineL’EtalonN-FrancebrusselssproutsMaximum1. 05.05.20043. 01.09.2004- 31.10.20040.07200.07200.07205005005000.0140.0140.01409.09.200416.09.200424.09.2004BBCH 48 sproutsproutsproutsproutsproutsprout<0.010.010.010.01<0.01<0.010.0420.0510.0750.0990.0980.130.0140.0230.0320.0450.0430.058<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0080.0860.1040.1370.1740.1710.2180*0371421formulation:100 ODRA-2066/05R 2005 0369/5D-59457 WerlWestönnenGermanybrusselssproutsCyrus1. 25.05.20053. 15.09.2005- 15.12.20050.0720.0720.0725005005000.0140.0140.01430.08.200513.09.200527.09.2005BBCH 47 sproutsproutsproutsproutsproutsprout0.010.010.020.01<0.01<0.010.0320.0360.0490.0290.0260.0240.0290.0380.0390.0300.0210.019<0.012<0.012<0.012<0.012<0.012<0.0120.0080.0090.0110.0080.0080.0080.0910.1050.1310.0890.0770.073-14-1103814formulation:150 OD- 301 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2066/05R 2005 0370/9F-27340Criquebeuf surSeineN-FrancebrusselssproutsAbacus1. 15.06.20053. 24.10.2005- 30.11.20050.0720.0720.0725005005000.0140.0140.01426.09.200510.10.200524.10.2005BBCH 46 sproutsproutsproutsproutsproutsprout0.010.010.010.01<0.010.010.0430.0410.0450.0350.0410.0410.0270.0230.0200.0200.0170.018<0.012<0.012<0.012<0.012<0.012<0.0120.0080.0080.0080.0080.0080.0080.1000.0940.0950.0850.0880.089-14-1103714formulation:150 ODRA-2066/05R 2005 0371/7D-53332BornheimGermanybrusselssproutsAbacus1. 24.05.20053. 01.10 2005- 15.12.20050.0720.0720.0725005005000.0140.0140.01422.09.200506.10.200520.10.2005BCH 49 sproutsproutsproutsproutsproutsproutsproutsprout0.010.010.02<0.010.010.010.010.010.0300.0330.0710.0570.0570.0640.0640.0600.0200.0250.0460.0230.0460.0340.0390.027<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0080.0120.0080.0080.008<0.0080.0080.0300.0800.0920.1570.1100.1330.1280.1330.139-14-110*0371421formulation:150 ODRA-2066/05R 2005 0372/5GB-IP17 3BSSaxmundhamUnitedKingdombrusselssproutsHelemus1. 27.05.20053. 15.12.2005- 31.01.20060.0720.0720.0725005005000.0140.0140.01418.11.200501.12.200516.12.2005BBCH 49 sproutsproutsproutsproutsproutsproutsproutsprout0.020.010.02<0.010.010.010.01<0.010.0320.0330.0590.0440.0530.0680.0620.0650.0120.0120.0120.0120.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0080.008<0.0080.008<0.008<0.008<0.008<0.0080.0840.0750.1110.0860.0950.1100.1040.107-15-110*0371421formulation:150 OD* Before the last treatment** Residues of each analyte calculated as spirotetramat (BYI 08330)- 302 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Annex I p: Summary of trial information – round cabbage, red cabbage and savoy cabbageApplication rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksField trials, Northern EuropeRA-2037/04R 2004 0152/3D-40764Langenfeld,GermanyroundcabbageAttraktion1. 30.06.20043. 15.10.20040.0720.0720.0726006006000.0120.0120.01220.09.200427.09.200404.10.2004BBCH 47 headheadheadheadhead0.010.130.010.01<0.010.0240.0250.0320.0370.0180.0240.0220.0230.0300.025<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.0080.0780.1970.0850.0970.0730*03714formulation:100 ODRA-2037/04R 2004 0156/6GB-PE22 7HGFrithville,UnitedKingdomredcabbageRococo1. 18.05.20043. 15.09.2004- 31.10.20040.0720.0720.0726006006000.0120.0120.01206.09.200413.09.200421.09.2004BBCH 47 headheadheadheadheadhead0.010.040.010.01<0.01<0.010.0650.0620.0600.0590.0620.0590.0130.0120.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0,012<0.008<0.008<0.008<0.008<0.008<0.0080.1080.1340.1020.1010.1040.1010*0361420formulation:100 ODRA-2037/04R 2004 0157/4F-80500FaverollesN-FranceSavoycabbageFirenza1. 10.05.20043. 01.11.2004- 15.12.20040.0720.0720.0725005005000.0140.0140.01426.10.200403.11.200409.11.2004BBCH 49 headheadheadheadheadhead<0.010.040.01<0.01<0.01<0.010.0120.0450.0170.0120.0120.0120.0350.0700.0440.0140.0120.013<0.012<0.012<0.012<0.012<0.012<0,012<0.0080.0080.008<0.008<0.008<0.0080.0770.1750.0910.056<0.0540.0550*0371421formulation:100 ODRA-2060/05R 2005 0352/0F-80480 DuryN-FranceredcabbageRondonF11. 15.06.20053. 01.10.2005- 10.10.20050.0720.0720.0725005005000.0140.0140.01424.08.200507.09.200521.09.2005BBCH 48 headheadheadheadheadheadheadhead<0.010.012<0.010.0220.010<0.01<0.01<0.010.0140.0190.0140.0200.0250.0250.0170.024<0.012<0.012<0.012<0.012<0.012<0,012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0,012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.0080.0560.0630.0560.0740.0670.0670.0590.066-14-110*0371421formulation:150 ODRA-2060/05R 2005 0353/9D-51399BurscheidGermanyredcabbageRoxy1. 10.05.20053. 15.09.2005- 15.11.20050.0720.0720.0725005005000.0140.0140.01430.08.200513.09.200527.09.2005BBCH 47 headheadheadheadheadhead0.036<0.010.038<0.01<0.01<0.010.010.0950.110.0920.0900.072<0.012<0.012<0.012<0.012<0.012<0,012<0.012<0.012<0.012<0.012<0.012<0,012<0.008<0.008<0.008<0.008<0.008<0.0080.0780.1370.1800.1340.1320.114-14-1103714formulation:150 OD- 303 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2060/05R 2005 0354/7D-42799LeichlingenGermanyroundcabbageGilson F11. 08.06.20053. 05.09.2005- 25.09.20050.0720.0720.0726006006000.0120.0120.01201.08.200515.08.20529.08.2005BBCH 45 headheadheadheadheadheadheadhead<0.01<0.01<0.010.0570.011<0.01<0.01<0.010.0320.0520.0400.0580.0610.0620.0530.0370.0440.0670.0710.0870.0940.0930.0990.074<0.012<0.012<0.012<0.012<0.012<0,012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.0080.1060.1490.1410.2220.1860.1850.1820.141-14-110*0371421formulation:150 ODRA-2060/05R 2005 0355/5D-59457 WerlWestönnenGermanyroundcabbageKingston1. 15.05.20053. 15.09.2005- 30.10.20050.0720.0720.0725005005000.0140.0140.01430.08.200513.09.200527.09.2005BBCH 48 headheadheadheadheadhead<0.01<0.01<0.01<0.01<0.01<0.010.0360.0350.0370.0240.0320.0260.0210.0220.0210.0140.0150.013<0.012<0.012<0.012<0.012<0.012<0,012<0.008<0.008<0.008<0.008<0.008<0.0080.0870.0870.0880.0680.0770.069-14-1103814formulation:150 ODRA-2060/05R 2005 0356/3D-42799LeichlingenGermanySavoycabbageRigolettoF11. 08.06.20053. 05.09.2005- 25.09.20050.0720.0720.0726006006000.0120.0120.01201.08.200515.08.200529.08.2005BBCH 45 headheadheadheadheadheadheadhead0.220.091<0.010.110.031<0.01<0.01<0.010.110.120.0760.0930.110.0640.0810.0550.0840.110.0660.110.100.0840.0740.068<0.012<0.012<0.012<0.012<0.012<0,012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.0080.4340.3410.1720.3330.2610.1780.1850.153-14-110*0371421formulation:150 ODRA-2060/05R 2005 0357/1F-80200EnnemainN-FrancesavoycabbageIce Prince1. 18.05.20053. 22.10.2005- 03.11.20050.0720.0720.0725005005000.0140.0140.01419.09.200503.10.200517.10.2005BBCH 48 headheadheadheadheadhead<0.010.0130.013<0.01<0.01<0.01<0.0120.0150.0240.0310.0260.027<0.012<0.0120.0280.0310.0210.018<0.012<0.012<0.012<0.012<0.012<0,012<0.008<0.008<0.008<0.008<0.008<0.008<0.0540.0600.0850.0920.0770.075-14-1103714formulation:150 ODRA-2060/05R 2005 0359/8D-51399BurscheidGermanysavoycabbageFirensa1. 10.05.20053. 15.09.2005- 15.11.20050.0720.0720.0725005005000.0140.0140.01416.08.200530.08.200513.09.2005BBCH 45 headheadheadheadheadhead0.380.240.30<0.01<0.01<0.010.130.120.100.0600.060.0420.130.0980.0810.0450.0610.054<0.012<0.012<0.012<0.012<0.012<0,012<0.008<0.008<0.008<0.008<0.008<0.0080.6600.4780.5010.1350.1510.126-14-1103714formulation:150 OD- 304 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksField trials, Southern EuropeRA-2038/04R 2004 0158/2E-08850 Gavá(Catalua)SpainredcabbageSombrero1. 20.11.20043. 25.04.2005- 20.05.20050.0720.0720.0726006006000.0120.0120.01211.04.200518.04.200525.04.2005BBCH 45 headheadheadheadheadhead<0.01<0.01<0.01<0.01<0.01<0.010.0980.110.150.190.170.140.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0,012<0.008<0.008<0.008<0.0080.0080.0080.1400.1520.1920.2320.2120.1820*0371423formulation:100 ODRA-2038/04R 2004 159/0I-70031 Andria(BA) (Puglia)ItalyroundcabbageHead StartF11. 15.09.20043. 25.11.2004- 25.12.20050.0720.0720.0728008008000.0090.0090.00911.11.200418.11.200425.11.2004BBCH 47 headheadheadheadhead0.010.070.01<0.01<0.010.0240.0390.0360.0510.0650.0120.0210.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.0080.0660.1500.0780.0930.1070*03714formulation:100 ODRA-2061/05R 2005 0350/4I-70031 AndriaItalyredcabbageZelox1. 20.08.20053. 20.12.2005- 20.01.20060.0720.0720.0728008008000.0090.0090.00924.11.200508.12.200522.12.2005BBCH 46 headheadheadheadheadheadheadhead0.041<0.01<0.010.030<0.01<0.01<0.01<0.010.0360.0250.0310.0470.0460.0580.0620.071<0.012<0.012<0.012<0.012<0.012<0,012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0,012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.0080.1090.0670.0730.1090.0880.1000.1040.113-14-110*0371421formulation:150 ODRA-2061/05R 2005 0351/2E-08840 GavaSpainroundcabbageGonzalesBlanca1. 01.09.20053. 28.11.2005- 28.12.20050.0720.0720.0725006006000.0140.0120.01228.10.200519.11.200505.12.2005BBCH 45 headheadheadheadheadhead0.010<0.01<0.01<0.01<0.01<0.010.0190.0220.0320.0290.0320.0340.0200.0180.0170.0170.0140.018<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0080.0690.0700.0790.0760.0760.082-16-1302714formulation:150 OD* Before the last treatment** Residues of each analyte calculated as spirotetramat (BYI 08330)- 305 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Annex I q: Summary of trial information – leafy brassicaApplication rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksField trials, Northern EuropeRA-2040/04R 2004 0164/7GB-CB2 5EUCambridgeUnitedKingdomcurly KaleDwarfGreeenCurled1. 21.06.20043. no data0.0720.0720.0725005005000.0140.0140.01426.10.200401.11.200407.11.2004BBCH 49 leaf, n.leaf, n.leaf, n.leaf, n.leaf, n.0.401.20.150.200.070.330.420.220.290.280.120.240.0810.110.080<0.012<0.012<0.012<0.012<0.0120.0080.0080.0080.0080.0120.8701.8800.4710.6200.4540*03815formulation:100 ODRA-2040/04R 2004 0165/5D-40789MonheimGermanycurly KaleWinterbor1. 16.06.20043. 15.09.20040.0720.0720.0725005005000.0140.0140.01424.08.200431.08.200407.09.2004BBCH 47 leaf, n.leaf, n.leaf, n.leaf, n.leaf, n.leaf, n.0.081.00.500.070.050.030.0700.230.120.0530.0500.0410.0940.180.120.0640.0480.037<0.012<0.012<0.012<0.012<0.012<0.0120.0120.0140.0130.0150.0200.0180.2681.4360.7650.2140.1800.138-10371420formulation:100 ODRA-2064/05R 2005 0367/9D-40789MonheimGermanycurly KaleWinterbor1. 25.05.20053.20.08.2005- 1.10.20050.07200.07200.07206006006000.0120.0120.01225.07.200508.08.200522.08.2005BBCH 48 leaf, n.leaf, n.leaf, n.leaf, n.leaf, n.leaf, n.leaf, n.leaf, n.1.20.900.0450.870.0860.0460.0290.0100.150.0790.0590.210.0920.0610.0620.0380.0550.0720.0190.0530.0420.0330.0210.014<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0080.010<0.0081.4251.0710.1431.1530.2400.1600.1340.082-14-110*0371421formulation:150 ODRA-2064/05R 2005 0368/7D-51399BurscheidGermanycurly KaleWinterbor1. 10.05.20053.15.09.2005-15.11.20050.07200.07200.07205005005000.0140.0140.01416.08.200530.08.200513.09.2005BBCH 78 leaf, n.leaf, n.leaf, n.leaf, n.leaf, n.leaf, n.1.10.911.10.0290.0200.0190.180.180.280.160.210.120.0510.0720.0750.0350.0510.022<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.0081.3511.1821.4750.2440.3010.181-14-1103714formulation:150 ODField trials, Southern EuropeRA-2041/04R 2004 0166/3F-86380OuzillyFrancechinesekaleOptiko1. 08.07.20043. 15.09.2004- 30.09.20040.07200.07200.07206006006000.0120.0120.01223.08.200430.08.200406.09.2004BBCH 43 leaf, n.leaf, n.leaf, n.leaf, n.0.380.110.01<0.010.370.280.190.150.110.120.0560.046<0.012<0.012<0.012<0.0120.0290.0340.0370.0390.9010.5560.3050.25703714formulation:100 OD- 306 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA -2041/04R 2004 0167/1E-08850 GavaSpainchinesekaleOnekilo1. 07.08.20043. 01.10.2004- 20.10.20040.07200.07600.07206006336000.0120.0120,01217.09.200423.09.200401.10.2004BBCH 47 leaf, n.leaf, n.leaf, n.leaf, n.leaf, n.leaf, n.0.100.470.080.07<0.01<0.010.280.500.380.310.380.250.0990.180.120.110.160.11<0.012<0.012<0.012<0.012<0.012<0.0120.0430.0540.0390.0430.0280.0300.5341.2160.6310.5450.5900.4120*0471420formulation:100 ODRA-2136/05R 2005 0709/7E-08840 GavaSpainchinesecabbageOne Kilo1. 01.09.20053. 20.10.2005- 15.11.20050.06600.07200.0720552100015000.0120.0070.00521.09.200505.10.200519.10.2005BBCH 46 headheadheadheadheadheadhead0.940.28<0.01<0.01<0.01<0.01<0.010.720.490.120.190.160.0820.0600.130.150.0470.0690.120.0680.055<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.0081.8100.9400.1970.2890.3100.1800.145-14-120271421formulation:150 ODRA-2136/05R 2005 0710/0I-70031 AndriaItalychinesecabbageTaranko1. 12.08.20053. 01.10.2005- 30.11.20050.07200.07200.07201000100010000.0070.0070.00714.09.200528.09.200512.10.2005BBCH 48 headheadheadheadheadheadheadhead0.048<0.01<0.010.020<0.01<0.01<0.01<0.010.110.160.110.110.130.150.130.130.0330.0280.0210.0290.0260.0320.0260.035<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.008<0.008<0.008<0.008<0.008<0.008<0.008<0.0080.2110.2180.1610.1790.1860.2120.1860.195-14-110*0371421formulation:150 ODleaf, n. = leaf, normal* Before the last treatment** Residues of each analyte calculated as spirotetramat (BYI 08330)- 307 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Annex I r: Summary of trial information – kohlrabiApplication rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksField trials, Northern EuropeRA-2043/04R 2004 0169/8D-59457 WerlWestönnenGermanykohlrabiKoist1. 27.04.20043. 05.06.2004- 15.6.20040.07200.07200.07204004004000.0180.0180.01806.05.200414.05.200421.05.20042ndappl.:BBCH 173rdappl.:BBCH 19cormleaf, n.cormleaf, n.cormleaf, n.cormleaf, n.cormleaf, n.cormleaf, n.0.010.040.031.20.010.660.010.06<0.01<0.01<0.01<0.010.420.410.552.10.521.20.510.730.330.100.130.0230.0640.110.110.480.120.290.0830.140.0200.0320.0120.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0080.0210.0080.0230.0080.027<0.0080.028<0.0080.017<0.0080.0140.5140.5930.7103.8150.6702.1890.6230.9700.3800.1710.1720.0710*0*00337714142121formulation:100 ODRA-2043/04R 2004 0170/1NL-1681 NDZwaagdijkOostNetherlandskohlrabiOlivia1. 08.06.20043. 25.07.2004- 25.08.20040.07200.07200.07206006006000.0120.0120.01213.07.200421.07.200428.07.20042ndappl.:BBCH 413rdappl.:BBCH 43cormleaf, n.cormleaf, n.cormleaf, n.cormleaf, n.cormleaf, n.cormleaf, n.<0.010.080.011.50.010.91<0.010.49<0.010.05<0.010.010.370.100.420.620.420.350.490.160.280.0410.200.0410.0320.0380.0380.210.0330.0970.0340.0590.0180.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0080.033<0.0080.042<0.0080.0420.0080.0560.0080.067<0.0080.0610.4320.2630.4882.3840.4831.4110.5540.7770.3280.1820.2420.1360*0*00337714142121formulation:100 OD- 308 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2065/05R 2005 0373/3D-40764LangenfeldReusrathGermanykohlrabiLech1. 25.04.20053.17.06.2005- 01.07.20050.07200.07200.07206006006000.0120.0120.01219.05.200503.06.200517.06.20052ndappl.:BBCH 433rdappl.:BBCH 46cormleaf, n.cormleaf, n.cormleaf, n.cormleaf, n.cormleaf, n.cormleaf, n.cormleaf, n.cormleaf, n.0.010.570.010.120.011.10.011.30.010.080.010.10<0.010.02<0.010.010.0960.870.220.180.150.420.130.410.190.140.150.0320.0940.0120.0450.0120.0130.280.0170.0620.0130.110.0130.120.0120.0440.012<0.0120.012<0.0120.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0080.022<0.0080.025<0.0080.022<0.0080.022<0.0080.038<0.0080.040<0.0080.032<0.0080.0290.1391.7540.2670.3990.1931.6640.1731.8640.2320.3140.1920.1960.1360.0880.0870.075-14-14-11-110*0*00337714142121formulation:150 ODRA-02065/05R 2005 0374/1D-51399BurscheidGermanykohlrabiAvanti F11. 10.05.20053. 20.07.2005- 30.08.20050.07200.07200.07201000100010000.0070.0070.00729.06.200513.07.200527.07.20052ndappl.:BBCH 423rdappl.:BBCH 47cormleaf, n.cormleaf, n.cormleaf, n.cormleaf, n.cormleaf, n.cormleaf, n.cormleaf, n.0.031.30.010.380.020.770.010.03<0.010.01<0.010.01<0.01<0.010.180.380.160.170.130.240.110.0270.110.0740.0880.0450.0680.0230.0150.0440.0140.0250.0120.0340.0120.0120.0120.0140.0120.0120.0120.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0080.0380.0080.0440.0080.054<0.0080.048<0.0080.062<0.0080.057<0.0080.0520.2451.7740.2040.6310.1821.110.1520.1290.1520.1720.130.1360.1100.109-14-14-11-110*0*0033771414formulation:150 OD* Before the last treatment** Residues of each analyte calculated as spirotetramat (BYI 08330)leaf, n. leaf, normal- 309 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Annex I s: Summary of trial information – green beansApplication rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksField trials, glasshouseRA-2042/04R 2004 0172/8I-00050PalidoroFiumicinoItalyclimbingFrenchbeanEmerite1. 02.04.20042. 21.05.20043. 04.06.2004- 30.06.20040.08640.12960.14400.1440600900100010000.0140.0140.0140.01414.05.200421.05.200428.05.200404.06.2004BBCH 71 bean w.pbean w.pbean w.p.bean w.p.bean w.p.bean w.p.0.030.240.130.060.060.040.170.260.250.110.120.0630.190.220.200.120.0810.042<0.0120.0120.0120.0120.0120.0120.0240.0300.0380.0250.0300.0230.4260.7620.6300.3270.3030.1800*07101421formulation:100 ODRA-2042/04R 2004 0173/6I-71043ManfredoniaItalyclimbingFrenchbeanBlue Lake1. 05.04.20042. 10.05.20043. 28.06.2004- 15.09.20040.14400.14400.14400.144010001000100010000.0140.0140.0140.01421.06.200428.06.200405.07.200412.07.2004BBCH 76 bean w.pbean w.pbean w.p.bean w.p.bean w.p.bean w.p.0.190.420.520.280.010.010.250.460.340.250.0660.0360.0770.120.0890.0760.0200.012<0.012<0.012<0.012<0.012<0.012<0.0120.0210.0250.0350.0290.0080.0080.5501.0370.9960.6470.1160.07800*07101421formulation:100 ODRA-2042/04R 2004 0174/4D-40764LangenfeldGermanyclimbingFrenchbeanMarkant1. 30.04.20042. 01.06.20043. 15.07.20040.14400.14400.14400.144010001000100010000.0140.0140.0140.01415.06.200422.06.200429.06.200406.07.2004BBCH 78 bean w.pbean w.pbean w.p.bean w.p.bean w.p.bean w.p.0.160.200.150.040.130.030.230.220.270.230.290.190.110.130.120.0990.0990.055<0.012<0.0120.0120.0120.0120.0120.0180.0180.0260.0210.0350.0320.5300.5800.5780.4020.5660.3190*07101421formulation:100 ODRA-2042/04R 2004 0175/2F-13870RognonasS-FranceclimbingFrenchbeanHelda1. 08.04.20042. 15.05.20043. 01.06.2004- 30.06.20040.12600.12600.12600.12608758758758750.0140.0140.0140.01419.05.200426.05.200402.06.200409.06.2004BBCH 79 bean w.pbean w.pbean w.p.bean w.p.bean w.p.bean w.p.0.100.280.220.350.150.040.0880.150.240.280.260.190.160.210.170.100.0990.0800.0120.0120.0120.0120.0120.0120.0240.0250.0330.0400.0430.0540.3840.6770.6750.7820.5640.3760*07101421formulation:100 ODRA-2042/04R 2004 0176/0I-00052FurbaraCerveteriItalyclimbingFrenchbeanEmerite1. 09.04.20042. 21.05.20043. 03.06.2004- 29.06.20040.08640.13680.14400.1440600950100010000.0140.0140.0140.01417.05.200424.05.200431.05.200407.06.2004BBCH 71 bean w.pbean w.pbean w.p.bean w.p.bean w.p.bean w.p.0.010.040.010.010.01<0.010.0410.0540.0490.0310.015<0.0120.100.100.110.0700.037<0.012<0.012<0.012<0.012<0.012<0.012<0.0120.0090.0100.0140.0120.008<0.0080.1720.2160.1950.1350.0820.0540*07101421formulation:100 OD- 310 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2042/04R 2004 0177/9I-70052MolfettaItalyclimbingFrenchbeanBlueLakes1. 03.04.20042. 15.05.20043. 15.06.2004- 20.07.20040.14400.14400.14400.144010001000100010000.0140.0140.0140.01426.05.200402.06.200409.06.200416.06.2004BBCH 74 bean w.pbean w.pbean w.p.bean w.p.bean w.p.bean w.p.0.010.080.020.010.01<0.010.0370.0820.0680.0460.0900.0260.0840.200.140.0750.0840.023<0.012<0.012<0.012<0.012<0.012<0.0120.0090.0090.0120.0090.0120.0080.1520.3830.2520.1520.2080.0790*07101421formulation:100 ODRA-2042/04R 2004 0178/7F-13550NovesS-FranceclimbingFrenchbeanDonna1. 12.04.20042. 20.05.20043. 05.06.2004- 30.06.20040.12600.12600.12600.12608758758758750.0140.0140.0140.01419.05.200426.05.200402.06.200409.06.2004BBCH 79 bean w.pbean w.pbean w.p.bean w.p.bean w.p.bean w.p.0.060.130.080.130.110.130.100.130.220.260.270.290.140.170.160.110.120.120.0120.0120.0120.0120.0120.0170.0200.0200.0270.0310.0430.0670.3320.4620.4990.5430.5550.6240*07101421formulation:100 ODRA-2042/04R 2004 0179/5D-40764LangenfeldGermanyclimbingFrenchbeanMarkant1. 30.06.20042. 01.08.20043. 01.09.2004- 30.09.20040.14400.14400.14400.144010001000100010000.0140.0140.0140.01411.08.200418.08.200425.08.200401.09.20o4BBCH 73 bean w.pbean w.pbean w.p.bean w.p.bean w.p.bean w.p.0.020.090.060.070.040.020.230.260.400.360.230.150.160.140.110.130.0980.0610.012<0.0120.0120.012<0.012<0.0120.0120.0120.0230.0220.0210.0150.4340.5140.6050.5940.4010.2580*07101421formulation:100 OD* Before the last treatment** Residues of each analyte calculated as spirotetramat (BYI 08330)bean w.p. bean with pod- 311 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Annex I t: Summary of trial information – hopApplication rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksField trials, Northern EuropeRA-2036/04R 2004 0148/5F-67160SchleithalN-FrancehopStrisselspalt3. 31.08.2004- 07.09.20040.1750.175220024000.0080.00727.04.200409.08.20041stappl.:BBCH 652ndappl.:BBCH 75cone, g.cone, g.cone, g.cone, KDcone, g.cone, KDcone, gcone, KD0.400.580.110.240.170.630.100.52<0.120.18<0.120.23<0.120.18<0.120.15<0.12<0.12<0.120.19<0.120.30<0.120.19<0.12<0.12<0.12<0.12<0.12<0.12<0.12<0.120.140.310.090.270.130.410.090.430.91.310.561.050.661.640.551.410*08814142222formulation:100 ODRA-2036/04R 2004 0149/3D-85283GebrontshausenGermanyhopHallertauerTradition1. 19932. 31.08.20043. 31.08.20040.1620.175230825000.0070.00727.07.200411.08.20041stappl.:BBCH68-892ndappl.:BBCH72-75cone,g.cone, g.cone, g.cone, KDcone, g.cone, KDcone g.cone, KD0.211.50.251.70.270.560.260.94<0.120.670.210.97<0.120.25<0.120.35<0.120.270.231.00.170.390.150.51<0.12<0.12<0.12<0.12<0.12<0.12<0.12<0.120.140.190.251.00.210.500.230.700.712.751.064.790.891.820.882.620*07714142222formulation:100 ODRA-2036/04R 2004 0150/7D-88069TettnangGermanyhopHallertauerMittelfrüh1. 19662. 30.08.20043. 30.08.20040.1750.175250025000.0070.00728.07.200410.08.20041stappl.:BBCH71-752ndappl.:BBCH75-77cone, g.cone g.cone, g.cone, KDcone, g.cone, KDcone g.cone, KDcone, g.0.140.980.432.00.191.10.251.20.260.310.880.271.1<0.120.750.140.580.20<0.120.240.341.40.140.750.160.600.17<0.12<0.12<0.12<0.12<0.12<0.12<0.12<0.12<0.120.210.390.381.60.261.30.301.20.460.92.611.546.220.834.020.973.71.210*0771414212128formulation:100 OD- 312 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Application rateper treatmentResidues**[mg/kg]*Report No.Trial NoLocationCommodity/VarietyDate of1. Sowing orplanting2. Flowering3. Harvestkg a.s./hawaterl/hakga.s./hlDates oftreatment(s)or no. oftreatmentand last dateGrowthstage atlasttreatmentor datePortionanalysedBYI08330BYI08330-enolBYI08330ketohydroxyBYI08330monohydroxyBYI08330enol-GlcTotalas BYI08330PHI[days]RemarksRA-2036/04R 2004 0151/5F-67210ObernaiN-FrancehopStrisselspalt1. 19982. 01.07.2004- 25.07.20043. 14.09.20040.1750.175220022000.0080.00810.08.200423.08.20041stappl.:BBCH 752ndappl.:BBCH 81cone, g.cone g.cone, g.cone, KDcone, g.cone, KDcone g.cone, KDcone, g.0.140.970.702.30.632.60.532.20.53<0.120.32<0.120.28<0.120.32<0.120.25<0.12<0.120.200.220.620.190.720.130.45<0.12<0.12<0.12<0.12<0.12<0.12<0.12<0.12<0.12<0.120.100.100.150.360.140.580.150.490.150.61.711.313.681.24.341.053.511.040*0881515222229formulation:100 ODRA -2108/05R 2005 0550/7D-85382GebrotshausenGermanyhopHallertauerTradition1. 19952. 01.07.20053. 02.09.20050.1500 2200 0.00711.08.2005 BBCH 82 cone, g.cone, g.cone, g.cone, KDcone, g.cone, KD0.850.280.151.50.110.930.240.12<0.120.19<0.120.21<0.12<0.12<0.12<0.12<0.12<0.12<0.12<0.12<0.12<0.12<0.12<0.12<0.080.080.080.080.080.081.410.720.592.010.551.460714142121formulation:150 ODRA-2108/05R 2005 0551/5F-67160SchleithalN-FrancehopStrisselspalt1. 01.06.19983. 01.09.20050.1500 2000 0.008 26.08.2005 BBCH 84 cone, g.cone, g.cone, g.cone, KDcone, g.cone, KD0.940.280.150.830.100.600.300.120.120.230.120.14<0.12<0.12<0.120.43<0.120.21<0.12<0.12<0.12<0.12<0.12<0.12<0.080.080.080.130.080.131.560.720.591.740.541.20713132020formulation:150 ODRA-2108/05R 2005 0552/3D-88069TettnangGermanyhopHallertauerMittelfrüh1. 19662. 10.07.20053. 31.08.20050.1500 2200 0.007 11.08.2005 BBCH75-82cone, g.cone, g.cone, KDcone, g.cone, KD0.980.321.50.211.10.360.120.320.120.31<0.120.170.880.120.52<0.12<0.12<0.12<0.12<0.12<0.080.080.290.080.331.660.813.110.652.38014142121formulation:150 ODRA-2108/05R 2005 0553/1F-67210ObernaiFrancehopStrisselspalt1. 19983.10.09.2005- 20.09.20050.1500 2000 0.008 30.08.2005 BBCH 86 cone, g.cone, g.cone, KDcone, g.cone, KD0.42<0.10.61<0.10.470.12<0.120.12<0.120.12<0.12<0.120.18<0.120.13<0.12<0.12<0.12<0.12<0.12<0.08<0.080.08<0.080.080.860.541.110.540.92014142121formulation:150 OD* Before the last treatment** Residues of each analyte calculated as spirotetramat (BYI 08330)cone, g. cone, greencone, KD cone, kiln-dried

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Annex II – Summary of trials conducted in NAFTA Reg ions

Residues were obtained using a modified version of the analytical method for determining the total spirotetramat residues (consisting of total residue s of spirotetramat, BYI 08330-enol, BYI 08330-ketoh ydroxy, BYI 08330-mono-hydroxy and BYI 08330-enol-Glc) in c rops (Method 00857).

The extraction of plant commodities to determine th e total spirotetramat residue involved blending a 5 -g sample with acetonitrile (ACN)/H 2 

### O (4:1) containing 0.02% (v/v) formic acid. Celite ® 

### was added, and the slurry was filtered. The filter cake was washed wi th additional extraction solvent, and the volume of the extract was adjusted to 50 mL with the extraction s olvent. An aliquot of a mixture of [ 13 

### C] isotopically labelled internal standards was added to a 2-mL aliquot of t he extract, and the sample was evaporated to near dryness. The sample was reconstituted with Millipo re water, and the aliquot was analyzed using HPLCMS/MS. The method was successfully validated by ana lysis of RACs spiked at 0.01 ppm, for each analyte in all matrices. Therefore the LOQ for each analyte i n all matrices was reported as 0.01 ppm.

All residues were corrected to spirotetramat parent equivalents for reporting purposes. The residues of all five analytes (greater than the respective analyte limit of detection) were summed to obtain the total spirotetramat residue for the sample. For the purp ose of calculating the total spirotetramat residue, individual analyte residues that were reported as < LOQ were assigned a finite value of the LOQ for tha t specific analyte.

CROP FIELD TRIALS ON POTATO PMRA # 1314451 GAP: Maximum seasonal rate of 175 g a.i./ha with a m inimum interval of 7 days between applications and a PHI of 7 days. Sixteen field trials were completed to investigate t he magnitude of total BYI 08330 residues in potatoes treated with two foliar applications of BYI 08330 150 OD or 240 SC. An appropriate number of trials were conducted in the NAFTA representative growing regions. Each formulation was applied at a rate of 0.086-0.092 kg a.i./ha with a re-treatment interval of 5 to 7 days for a total seasonal applic ation rate of 0.173-0.180 kg a.i./ha. All applicatio ns were made using spray volumes of 121 to 191 L/ha and Dyne-Amic (0.5% v/v) as an adjuvant. Potato tubers were harvested 7 days after the last application. Decline experiments were perf ormed at two different sites in order to ascertain changes in the magnitude of residues with time. The total residues of spirotetramat declined when the PHI increased fr om 3 to 20 days, but it was only observed at one site. Total spirot etramat residues were higher with the 150 OD formul ation in comparison

to the 240 SC formulation. Total Spirotetramat Residue Levels (ppm) Commodity Total Rate

(kg a.i./ha) PHI

(days) n Min. Max. HAFT Median Mean SD

Potato -150 OD 7 32 <0.050 0.457 0.450 0.119 0.171 0 .125

Potato -240 SC 0.173-

0.180 7 8 <0.060 0.139 0.138 0.075 0.087 0.032

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

CROP FIELD TRIALS ON BRASSICA LEAFY VEGETABLES PMRA #1314488 GAP: Maximum seasonal rate of 175 g a.i./ha with a m inimum interval of 7 days between applications and a PHI of 1 day. A total of twenty field trials were conducted in rep resentative commodities of crop subgroup 5A (broccol i (3), cauliflower (3), and cabbage (6) and subgroup 5B (mustard greens (8)). A decline trial was conducted with broccoli, cabbage and mustard greens. An appropriate number of trials we re conducted in the NAFTA representative growing regi ons. BYI 08330 100 OD or BYI 08330 240 SC were applied at targ et rates of 88 g a.i./ha/application at intervals o f 5-7 days for a total seasonal application rate of 171-184 g a.i./h a (BYI 08330 100 OD) and 174-176 g a.i./ha (BYI 08330 240 SC). All applications were made using spray volumes of 102 t o 188 L/ha and Dyne-Amic (0.5% v/v) as an adjuvant. Total residues of spirotetramat were generally higher in commoditi es treated with the 100OD formulation in comparison to the 240SC

formulation.There was no clear decline of total BYI 08330 residues in broccoli/cauliflower treated with either the 100OD or 240SC formulated products. Decline of total BYI 08330 residues was only observed in cabbage heads with w rapper leaves treated with the 100OD formulation. Total BYI 08330 residues in mustard greens declined with tim e when treated

with the 240SC formulation. Total Spirotetramat Residue Levels (ppm) Commodity Total Rate

(kg a.i./ha) PHI

(days) n Min. Max. HAFT Median Mean SD

Broccoli/Cauliflower

100OD

0.173 -0.177 1 13 0.099 0.451 0.423 0.369 0.336 0.110 Flower head

and stems 240 SC

0.176 1 4 0.210 0.325 0.307 0.289 0.278 0.048

Cabbage

100OD

0.173-0.177 1 12 0.054 0.924 0.911 0.312 0.394 0.317 Heads with

wrapper leaves 240 SC

0.176 1 2 0.050 0.050 0.050 0.050 0.050 NA

100OD

0.173-0.177 1 10 0.052 0.170 0.164 0.095 0.097 0.041 Heads with out wrapper

leaves 240 SC

0.176 1 2 0.055 0.056 0.056 0.056 0.056 NA

Mustard Greens

100 OD

0.171- 0.184 1 17 0.771 5.490 5.358 3.378 2.795 1.708

Greens 240 SC

0.174 -0.176 1 4 0.784 4.460 4.400 2.600 2.611 2.066

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

CROP FIELD TRIALS ON CUCURBIT VEGETABLES PMRA # 1314489

GAP: Maximum seasonal rate of 175 g a.i./ha with a m inimum interval of 7 days between applications and a PHI of 1 day.

A total of 17 field trials were conducted in represe ntative commodities of crop group 9 (cucumber, musk melon and summer squash). An appropriate number of trials were conducted in the NAFTA representative growing region s. Two broadcast foliar applications of either BYI 08330 10 0 OD or BYI 08330 240 SC were applied at a target ra te of 88 g a.i./ha/application, with a re-treatment interval o f 5-7 days. Total seasonal application rates for a ll trials ranged from 165 to 181 g a.i./ha for BYI 08330 100 OD and from 173 to 179 g a.i./ha for BYI 08330 240 SC. All spray mixt ures included Dyne-Amic (0.5% v/v) as an adjuvant. Samples of each commodities were collected one day after the last application. In the decline trials, samples were collected at five intervals corresponding to PHIs of approximately 0, 1, 3, 7 and 10 days. Total spirotetramat residue levels were similar in cucumbers and muskmelons treated with the 100OD or 240SC formulations. However, total spirotetramat residues were higher in summer squash treated with the 100O D formulation. There was no apparent decline of residues in cucumb er and muskmelon. However, a decline of residues wa s observed in summer squash when treated with the OD formulation from a 1 day PHI to a 7 day PHI. Total Spirotetramat Residue Levels (ppm) Commodity Total Rate

(kg a.i./ha) PHI

(days) n Min. Max. HAFT Median Mean SD

Cucumber -

100 OD 0.165-0.181 1 12 <0.050 0.076 0.075 0.050 0.057 0.011

Cucumber -

240 SC 0.173-0.179 1 4 <0.050 0.057 0.054 0.050 0.052 0

Muskmelon100 OD 0.165-0.181 1-2 12 <0.050 0.134 0.098 0.054 0.063 0.024

Muskmelon -

240 SC 0.173-0.179 1-2 4 <0.050 0.163 0.113 0.060 0.083 0.053

Summer Squash-100

OD 0.165-0.181 1 10 <0.050 0.184 0.173 0.069 0.095 0.051

Summer Squash - 240

SC 0.173-0.179 1 2 <0.050 0.051 0.051 -- -- --

CROP FIELD TRIALS ON LEAFY VEGETABLES PMRA # 1314487 GAP: Maximum seasonal rate of 175 g a.i./ha with a m inimum interval of 7 days between application and a PHI of 3 days.

A total of 24 field trials were conducted in order t o investigate the magnitude of total BYI 08330 resid ues in/on representative commodities of crop group 4 (head an d leaf lettuce, celery, and spinach). An appropriate number of trials were conducted in the NAFTA representative growing re gions.Trials were conducted with either a 100 OD fo rmulation or a 240 SC formulation being applied twice at a target r ate of 88 g a.i./ha with 5 to 8 days interval betwe en treatments. The total seasonal application rate was 0.171 – 0.183 g a.i./ha. All applications were made using spray v olumes of 83 to 189 L/ha and Dyne-Amic (0.5%) as an adjuvant. Samples of head lettuce, leaf lettuce, celery and spinach wer e harvested 3 days after the last treatment. In the decline trial s, samples were collected at 0, 1, 3, 7, and 10-day PHIs. Total spirotetramat residues declined with increasing PHIs in head lettuce, leaf lettuce, celery and spinach. Residues were higher in leaf lettuce, celery and spinach when tre ated with the 100 OD formulation. Residue levels we re similar in head lettuce (with and without wrapper leaves) when trea ted with the 100 OD or 240 SC formulated products.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Total Spirotetramat Residue Levels (ppm) Commodity Total Rate

(kg a.i./ha) PHI

(days) n Min. Max. HAFT Median Mean SD

3 (with wrapper leaves) 12 0.197 0.918 0.822 0.708 0.605 0.261

Head Lettuce 0.171-0.183

100 OD 3 (without

wrapper leaves) 10 0.111 0.385 0.383 0.167 0.203 0.101

3 (with wrapper leaves) 4 0.173 1.035 0.957 0.583 0.593 0.427 Head Lettuce 0.171-0.181

240 SC 3 (without

wrapper leaves) 4 0.160 0.241 0.234 0.224 0.212 0.036

0.171-0.183

100 OD 3 12 0.188 1.676 1.604 0.831 0.882 0.449

Leaf Lettuce 0.171-0.181

240 SC 3 2 0.211 0.227 0.219 0.219 0.219 NA

0.171-0.183

100 OD 3 15 0.248 2.633 2.533 0.606 1.019 0.856 Celery 0.171-0.181

240 SC 3 4 0.402 0.490 0.465 0.424 0.435 0.040

0.171-0.183

100 OD 3 14 0.204 3.360 3.071 1.334 1.493 0.977 Spinach 0.171-0.181

240 SC 3 2 2.338 2.654 2.496 2.496 2.496 NA

CROP FIELD TRIALS ON CITRUS FRUITS PMRA #1314490 US GAP: Two foliar sprays at 0.18 kg a.i./ha/applicat ion with a minimum retreatment interval of 21 days, for a maximum seasonal rate of 0.36 kg a.i./ha and a PHI of 1 day. During the 2005 growing season, trials were conduct ed on representative commodities of crop group 10 ( orange, lemon, grapefruit). An appropriate number of trials were c onducted in the NAFTA representative growing regions. Two groundbased airblast spray applications of either BYI08330 150 OD or BYI08330 240 SC were made at rates that ra nged from 0.168 to 0.187 kg a.i./ha/application, for a total seasonal rate of from 0.344 to 0.360 kg a.i./ha/sea son. The interval between applications ranged from 14 to 21 days. All spray mixtures included Dyne-Amic adjuvant (0.25% v/ v). Samples of oranges, lemons and grapefruits were harvested at a preharvest interval (PHI) of 1 day. In decline tria ls, samples were collected at five intervals corresponding to PHIs of 0, 1, 7, 10, and 14 days. Additional orange samples were collected to determine the effect of peeling. Most of the residu es in oranges appeared to be associated with the pe el since the levels decreased to below the LOQ when the peel was remove d. Total spirotetramat residue levels were similar in commodities

treated with the BYI 08330 150 OD formulation and th e BYI 08330 240 SC formulation. However, total spirot etramat residues (maximum values) were higher in commoditie s treated with the concentrated spray. In decline t rials, detectable residues dissipated slightly with increasing PHIs in orange, with no apparent decline in grapefruit and lemon. Total Spirotetramat Residue Levels (ppm) Commodity Total Rate (kg a.i./ha) PHI

(days) n Min. Max. HAFT Median Mean SD

Orange -150 OD 1 51 0.250 0.433 0.427 0.298 0.306 0 .054 Orange -240 SC 0.344–0.360 1 6 0.250 0.413 0.388 0.307 0.315 0.064

Lemon -150 OD 1 20 0.251 0.465 0.456 0.300 0.321 0. 063

Lemon -240 SC 0.344–0.360 1 2 0.305 0.392 0.348 — — — Grapefruit -150 OD 1 24 0.250 0.351 0.344 0.250 0.2 60 0.027 Grapefruit -240 SC 0.344–0.360 1 4 0.250 0.250 0.250 0.250 0.250 0

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

CROP FIELD TRIALS ON FRUITING VEGETABLES PMRA #1314516 GAP: Maximum seasonal rate of 175 g a.i./ha with a m inimum interval of 7 days between applications and a PHI of 1 day. A total of 21 trials were conducted in or on represe ntative commodities of crop group 8 (tomatoes, bell and non-bell peppers). An appropriate number of trials were cond ucted in the NAFTA representative growing regions. At each test location, two broadcast foliar applications of BYI08 330 100 OD or BYI08330 240 SC were made to tomatoes, bell peppers, or chili peppers at a target rate of 88 g a.i./ha/a pplication for a total seasonal rate that ranged fr om 0.168 to 0.199 kg a.i./ha. Retreatment intervals were 5 to 7 days wit h a preharvest interval of 1 day. All spray mixtures included Dyne-Amic adjuvant. Total spirotetramat residue levels were h igher in fruiting vegetables treated with the 100OD formulation in comparison to the 240SC formulation. In decline stud ies, samples were collected at PHIs of 0, 1, 3, 7 an d 10 days. There

was no clear trend of decline observed in the total spirotetramat residues (maximum values) in tomato, bell pepper, or nonbell pepper. Total Spirotetramat Residue Levels (ppm) Commodity Total Rate

(kg a.i./ha) PHI

(days) n Min. Max. HAFT Median Mean Std. Dev.

Tomato-100

OD 1 24 0.060 0.227 0.214 0.137 0.139 0.049

Tomato-240 SC 0.168–0.199

1 6 0.072 0.189 0.177 0.139 0.130 0.048 Bell pepper-100

OD 0.168–0.199 1 12 0.156 0.682 0.655 0.299 0.351 0.18 2

Bell pepper-240

SC 0.168–0.199 1 4 0.188 0.361 0.275 0.259 0.267 0.080

Chili pepper100 OD 0.168–0.199 1 6 0.427 1.379 1.232 0.558 0.748 0.390

CROP FIELD TRIALS ON GRAPES PMRA #1314622 GAP: Maximum seasonal rate of 220 g a.i./ha with a m inimum interval of 30 days between applications and a PHI of 7 days. A total of 12 trials were conducted on grapes durin g the 2005 growing season. An appropriate number of trials were conducted in the NAFTA representative growing regions .Test substance BYI 08330-150 OD or 240 SC was applie d as a ground-based foliar spray at rates that ranged from 0.109 to 0.114 kg a.i./ha/application. The interva l between applications ranged from 28 to 30 days. Total seasonal applicati on rates for all trials ranged from 0.219 to 0.227 kg a.i./ha. All aplications were made in spray volumes of 458 to 65 4 L/ha and used Dyne-Amic (0.25% v/v) as an adjuvant . Samples were collected 7 days after the last application. In a d ecline trial, grapes treated with the 150 OD formul ation were collected at five intervals corresponding to PHIs of 3, 7, 10, 14 , and 21 days. Total spirotetramat residues were hi gher with the 150 OD formulation in comparison to the 240 SC formulation. Total spirotetramat residues did not appear to dis sipate when the PHI increased from 3 to 21 days. Total Spirotetramat Residue Levels (ppm) Commodity Total Rate

(kg a.i./ha) PHI

(days) n Min. Max. HAFT Median Mean Std. Dev. Grape- 150 OD 0.219–0.227 7 24 0.109 1.290 1.024 0.329 0.406 0.257 Grape- 240 SC 0.219–0.227 7 6 0.187 0.547 0.466 0. 347 0.348 0.130

### - 318 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

CROP FIELD TRIALS ON HOPS PMRA # 1314494 GAP: Maximum seasonal rate of 220 g a.i./ha with a m inimum interval of 14 days between applications and a PHI of 7 days. Three field trials were conducted during the 2005 g rowing season. An appropriate number of trials were conducted in the NAFTA representative growing regions. At each test loc ation, BYI08330 150 OD or BYI08330 240 SC was applied twice as a postemergent foliar spray at a rate of 0.108 to 0 .112 kg a.i./ha/application with a retreatment inte rval of 12 to 14 days. The total application rate was from 0.218 to 0.224 kg a.i./ha/season. All spray mixtures included Dyne- Amic (0.25% v/v) as an adjuvant. Hop cones were harvested at preharvest interval of 7 days. Decline trials were conducted with samples collected at 7 and 14 days after the last applicati on.Total spirotetramat residues were higher with th e 150 OD formulation in comparison to the 240 SC formulation. Total spirotet ramat residues declined slightly when the PHI increa sed from 7 to 14 days. Total Spirotetramat Residue Levels (ppm) Commodity Total Rate

(kg a.i./ha) PHI

(days) n Min. Max. HAFT Median Mean Std. Dev. Hops- 150 OD 0.218–0.224 7 6 2.164 5.820 5.492 5 .167 4.427 1.675 Hops- 240 SC 0.218–0.224 7 2 3.149 4.512 3.830 — — — CROP FIELD TRIALS ON POME FRUITS PMRA # 1314492 GAP: Maximum seasonal rate of 440 g a.i./ha with a m inimum intervalof 14 days between applications and a PHI of 7 days. A total of 18 field trials were conducted on the rep resentative commodities of crop group 11 (apples an d pears) during the 2005 growing season. An appropriate number of trial s were conducted in the NAFTA representative growing regions. Applications of spirotetramat were made with one of two end-use products, BYI 08330 150OD or BYI 08330 24 0SC. Applied rates were 0.155 to 0.167 kg a.i./ha for the first application and 0.134 to 0.145 kg a.i./ha fo r the second and third applications, for a total of 0.430 to 0.447 kg a.i. /ha/season with a 14 day re-treatment interval. All spray mixtures included Dyne-Amic adjuvant. Apples and pears were collected 7 days following the final application. Decline tria ls were conducted on apples and pears with samples collected at pre-h arvest intervals of 0, 7, 14 and 21 days. Total spi rotetramat residues were higher in apples and pears treated with the 15 0OD formulation. However, total spirotetramat resid ues were not significantly different between the application spr ay volumes (concentrated and dilute). Total spirote tramat residues in/on pome fruit declined with time. Total Spirotetramat Residue Levels (ppm) Commodity Total Rate

(kg a.i./ha) PHI

(days) n Min. Max. HAFT Median Mean Std. Dev. Apple-150 OD 0.430–0.447 7 44 0.052 0.375 0.344 0.12 6 0.148 0.090 Apple-240 SC 0.430–0.447 7 6 0.062 0.144 0.143 0.075 0.094 0.039

Pear-150 OD 0.430–0.447 7 22 0.063 0.373 0.344 0.175 0.177 0.086

Pear-240 SC 0.430–0.447 7 4 0.137 0.259 0.250 0.196 0 .197 0.062

CROP FIELD TRIALS ON STONE FRUITS PMRA #1314485 GAP: Maximum seasonal rate of 270 g a.i./ha with a m inimum intervalof 14 days between applications and a PHI of 7 days. A total of 21 trials were conducted on the represen tative commodities of crop group 12 (cherries, peac hes, plums). An appropriate number of trials were conducted in the NAFTA representative growing regions. At each test loc ation, two airblast spray applications of BYI08330 150OD or BYI 08330 240SC were made at rates from 0.156 to 0.165 k g a.i./ha/application for the first application and 0 .107 to 0.112 kg a.i./ha/application for the second application for a total seasonal rate that ranged from 0.265 to 0.274 kg a. i./ha. All spray mixtures included the adjuvant Dyne -Amic (0.25% v/v).The retreatment interval was 12 to 15 days wit h a pre-harvest interval of 7 days. Decline trials were conducted with each commodity and the samples were collected at PHI s of 0, 7, 10, 14 and 21 days. Total spirotetramat residues were higher in cherries, peaches and plums treated with the 150OD compared to the 240 SC formulated products . The maximum total residues in plums were higher when tr eated with the concentrated spray. Total spirotetra mat residues declined with increasing PHIs in cherries, but not i n peaches or plums.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Total Spirotetramat Residue Levels (ppm) Commodity Total Rate (kg a.i./ha) PHI

(days) n Min. Max. HAFT Median Mean Std. Dev.

0.265-0.274

Concentrated 7 12 0.318 2.120 2.016 1.315 1.266 0.548

Cherries – 150OD 0.265-0.274

Dilute 7 12 0.222 2.127 2.044 1.602 1.480 0.564

Cherries- 240SC 0.265-0.274

Concentrated 7 2 0.572 0.645 0.608 0.608 0.608 -

0.265-0.274

Concentrated 7 24 0.273 1.227 1.034 0.432 0.496 0.211 Peaches –

150OD 0.265-0.274

Dilute 7 14 0.414 1.142 1.109 0.692 0.692 0.217

Peaches – 240SC 0.265-0.274

Concentrated 7 6 0.339 0.809 0.668 0.560 0.539 0.178

0.265-0.274

Concentrated 7 12 0.059 0.373 0.306 0.225 0.237 0.107

Plum – 150OD 0.265-0.274

Dilute 7 12 0.091 0.842 0.683 0.212 0.313 0.243

Plum – 240SC 0.265-0.274

Concentrated 7 2 0.060 0.065 0.062 0.062 0.062 -

CROP FIELD TRIALS ON TREE NUTS PMRA #1314621 GAP: Maximum seasonal rate of 380 g a.i./ha with a m inimum interval of 14 days between applications and a PHI of 7 days. Ten field trials were conducted on the representati ve commodities of crop group 14 (almonds and pecans ). An appropriate number of trials were conducted in the NAFTA represen tative growing regions. At each test location, three ground based airblast spray applications of either BYI08330 150 O D or BYI08330 240 SC were made to tree nuts at rates that ranged from 0.155 to 0.162 kg a.i./ha/application for the first application, and from 0.107 to 0.114 kg a.i./ ha/application for the second and third applications. Total seasonal appli cation rates ranged from 0.369 to 0.386 kg a.i./ha with application intervals of 12 to 20 days and a preharvest interva l of 7 days. All spray mixtures included Dyne-Amic (0 .25% v/v) as an adjuvant. Decline trials were conducted with sample s collected at 0, 6, 10, 13 and 21 days after the l ast application. Total spirotetramat residue levels were higher in tree nu ts treated with the 150 OD formulation. However, th ere was no significant difference observed in total spirotetra mat residues in tree nuts treated with concentrated or dilute spray volumes. Residues did not decline in almond or peca n nutmeat with increasing PHIs. Total Spirotetramat Residue Levels (ppm) Commodity Total Rate (kg a.i./ha) PHI

(days) n Min. Max. HAFT Median Mean Std. Dev.

Almond nutmeats150 OD 7 20 0.050 0.143 0.128 0.075 0.081 0.031

Almond nutmeats240 SC 0.369–0.386

7 4 0.063 0.083 0.078 0.072 0.072 0.008

Almond Hulls150 OD 7 20 1.261 5.145 4.988 2.466 2.931 1.333

Almond Hulls- 240

SC 0.369–0.386

7 4 1.923 5.260 4.579 2.919 3.255 1.627

Pecans- 150 OD 7 20 0.050 0.297 0.295 0.053 0.105 0. 087

Pecans- 240 SC 0.369–0.386 7 2 0.052 0.078 0.065 — — —

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Annex III – Calculations of MRLs with NAFTA Calcula tor

General Considerations:

The applicant is requesting registration for both S C and oil-dispersion (OD) formulations, along with different spray volume (concentrated and dilute). All of the field trials employed application with the OD form ulation (100 OD or 150 OD) with side-by-side comparisons wi th the SC formulation (240 SC) conducted at a few locations for each of the proposed crops. The resu lting data indicated that for some of the tested cr ops, residues were greater following application of the OD formulations as compared to the SC formulation; for the remaining crops, a relationship between formula tion and residues was not discernable. It was determined that the SC residue data should be exclu ded from all MRL calculations as it is derived from a different distribution that of the OD residue data. However, in those cases where the SC formulation resulted in higher residues than the OD formulation, the SC data was included in the MRL calculations. As spec ified by the “ Guidance for Setting Pesticide Tolerances Based on Field Trial Data SOP”, the field trial application rates and PHIs must be within 25% of the maximum la bel application rate and minimum label PHI, respectively to be included. However, when the tot al residue of spirotetramat at earlier or later int ervals (PHIs) exceeded the total residue at the critical G AP, then the higher values were evaluated to cover the worst case residue. The residue values consisted of the total of spirotetramat, BYI 08330-enol, BYI 08 330- ketohydroxy, BYI 08330-mono-hydroxy and BYI 08330-e nol-Glc, as parent equivalents.

MRL calculations were conducted on all representati ve crops of a crop group and the highest MRL output was used to determine the MRL for the crop group. T he rounding procedure was done as outlined in the

“ Guidance for Setting Pesticide Tolerances Based on Field Trial Data SOP”.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

TABLE XX Proposed MRL Values for Spirotetramat

RAC EP PHI (days) Vol (L/ha) n min

(ppm) max (ppm) median (ppm) mean (ppm) NAFTA

MRL (ppm) EU-MRL

(ppm) Calc.

Method NAFTA

Rate (g a.i./ha) EU Rate

(g a.i./ha)

Broc/Cauli 100 OD 1 102 to 188 13 0.099 0.45 0.37 0.34 0.70 1 Cal 177 72 Cabbage WW 100 OD 1 102 to 188 12 0.05 0.92 0.31 0.39 2.5 0.5 UClmed 177 72 Cabbage NW 100 OD 1 102 to 188 10 0.05 0.17 0.09 0.10 0.25 0.5 NAFTA I 177 72

Mustard 100 OD 1 102 to 188 17 0.77 5.5 3.38 2.80 8.0 Cal 187 72 Crop Group MRL CG5A = 1.0 ppm CG5B = 8.0 ppm

Orange 150 OD 1 375–653 27 <0.25 0.43 0.32 0.32 0.60 0.5 Cal 360 288

Lemon 150 OD 1 375–653 10 0.277 0.46 0.35 0.35 0.60 0.5 NAFTA I 360 288 grapefruit 150 OD 1 375–653 12 <0.25 0.34 0.25 0.27 0.40 0.5 Cal 360 288 Crop Group 10 MRL 0.60

Cucumber 100 OD 1 102–184 13 0.05 0.08 0.05 0.06 0.09 0.2 Cal 181 72

Muskmelon SC 1-2 140–183 4 0.05 0.16 0.06 0.08 0.17 0.2 Rounding 179 72 Squash 100 OD 1 102–184 11 0.05 0.18 0.06 0.09 0.30 NAFTA I 181 Crop Group 9 MRL 0.30

tomato 100 OD 1 101–182 24 0.06 0.23 0.14 0.14 0.35 2 green NAFTA I 199 144 grhs Pepper 100 OD 1 101–182 12 0.16 0.68 0.30 0.35 1.1 2 NAFTA I 199 144 Cayenne 100 OD 1 101–182 6 0.43 1.4 0.56 0.75 2.5 NAFTA I 199 Crop Group 8 MRL 2.5 ppm

Grape 150 OD 7 458–654 24 0.11 1.3 0.33 0.41 1.3 1 NAFTA I 227 96

Hops 150 OD 7 458–654 6 2.2 5.8 5.2 4.4 10 10 Cal 224 150--300

Lettuce head 100 OD 3 83–189 12 0.20 0.92 0.71 0.60 1.4 5 Cal 183 72

Lettuce inner 100 OD 3 83–189 10 0.11 0.38 0.17 0.20 0.60 5 NAFTA I 183 72

Leaf lettuce 100 OD 3 83–189 12 0.19 1.7 0.83 0.88 2.5 Cal 183 72 Celery stalk 100 OD 3 83–189 15 0.25 2.6 0.61 1.0 4.5 NAFTA I 183 72 Spinach 100 OD 3 83–189 14 0.20 3.4 1.3 1.5 9.0 NAFTA I 183 72 Crop Group 4 MRL CG = 9.0

Apple 150 OD 7 327–654 24 0.052 0.37 0.13 0.15 0.50 0.3 NAFTA I 447 216

Pear 150 OD 7 327–654 12 0.08 0.41 0.20 0.20 0.70 0.3 NAFTA I 447 216 Crop Group 11 MRL 0.70 ppm

Potato (1C) 150 OD 7 121–191 34 0.05 0.46 0.12 0.17 0.60 NAFTA I 180

Cherry 150 OD 7 365–681 12 0.32 2.1 1.3 1.3 4.5 2 NAFTA I 274 216

Peach 150 OD 7 1960–3662 22 0.27 1.1 0.56 0.62 1.4 2 NAFTA I 274 216

Plum 150 OD 7 1960–3662 12 0.09 0.84 0.21 0.31 1.5 2 NAFTA I 274 216 Crop Group 12 MRL CG = 4.5 ppm

Almond nut 150 OD 7 337–634 10 0.05 0.14 0.08 0.09 0.25 NAFTA I 386

Pecan 150 OD 7 1883–2865 10 0.05 0.30 0.05 0.12 0.25 (MLE) Cal 386 Crop Group 14 MRL CG=0.25 ppm

### - 322 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Leafy Brassica

Greens (5A); Head and Stem Brassica (5B)

The dataset used to establish an MRL for spirotetra mat in/on Head and Stem Brassica, subgroup 5A consisted of cabbage field trial data representing application rates of 0.172- 0.177 kg a.i./ha (heads with wrapper leaves, 100 OD formulation) with a 1-day PH I. All 12 field trial sample results were above th e combined LOQ of 0.05 ppm. Since there were no valu es (combined residues) reported below the LOQ, maximum-likelihood estimation (MLE) procedures were not needed to impute censored values. Visual inspection of the lognormal probability plot provid ed in the spreadsheet indicates that the dataset is reasonably lognormal. The result from the approxim ate Shapiro-Francia test statistic confirmed that t he assumption of lognormality should not be rejected. Based on the 95% UCL on the 95 th 

### percentile and the point estimate of the 99 th 

### percentile, the value is rounded to 2.5 ppm. Ther efore, 2.5 ppm is the recommended MRL level for spirotetramat in/on Head and Stem Brassica ( subgroup 5A).

The dataset used to establish an MRL for spirotetra mat in/on Leafy Brassica Greens , subgroup 5B consisted of mustard greens field trial data repres enting application rates of 0.171- 0.1864 kg a.i./h a(100 OD formulation) with a 1-day PHI. All 17 field trial sample results were above the combined LOQ of 0.05 ppm. Since there were no values (combined residues) repo rted below the LOQ, MLE procedures were not needed to impute censored values. Visual inspection of the lognormal probability plot provided in the spreads heet indicates that the dataset is not lognormal. The r esult from the approximate Shapiro-Francia test sta tistic confirmed that the assumption of lognormality shoul d be rejected. Using the CA Method and the μ + 3 σ , the value rounds to 8.0 ppm. Therefore, 8.0 ppm is the recommended MRL level for spirotetramat in/on Leaf y Brassica greens, subgroup 5B.

CABBAGE

Regulator: Cabbage 100OD phi 1

Chemical:

Crop:

PHI:

App. Rate: Submitter:

n: 12

min: 0.05

max: 0.92 median; 0.31

average: 0.39

95th Percentile 99th Percentile 99.9th Percentile

EU Method I 1.0 1.2 1.4

Normal (1.3) (1.6) (--)

1.5 3.0 7.0

(4.5) (12) (--)

1.3

1.4

UPLMedian 95th 2.5

0.9426 p-value > 0.05 : Do not reject lognormality assumpt ion EU Method I Log Normal

EU Method II

Distribution-Free

California Method

μ + 3 σ

Approximate Shapiro-Francia Normality Test

### - 323 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

MUSTARD GREENS

Citrus

The dataset used to establish an MRL for spirotetra mat in/on citrus fruit, group 10 consisted of lemon field trial data representing application rates of 0.343- 0.360 kg a.i./ha (concentrated spray, 100 OD formul ation) with a 1-day PHI. All 10 field trial sample result s were above the combined LOQ of 0.05 ppm. Since t here were no values (combined residues) reported below t he LOQ, MLE procedures were not needed to impute censored values. Visual inspection of the lognormal probability plot provided in the spreadsheet indic ates that the dataset is reasonably lognormal. The resu lt from the approximate Shapiro-Francia test statis tic confirmed that the assumption of lognormality shoul d not be rejected. Using the lognormal EU Method I and the point estimate of the 95 th 

### percentile, the value is rounded to 0.60 ppm. The refore, 0.60 ppm is the recommended MRL level for spirotetramat in/on citru s fruit (group 10). Regulator: Mustard 100OD phi 1

Chemical:

Crop:

PHI:

App. Rate:

Submitter:

n: 17

min: 0.77

max: 5.49 median; 3.38

average: 2.80

95th Percentile 99th Percentile 99.9th Percentile

EU Method I 6.0 7.0 9.0

Normal (8.0) (9.0) (--)

8.0 13 25

(15) (30) (--)

9.0

8.0

UPLMedian 95th 25

0.8789 0.05 >= p-value > 0.01 : Reject lognormality assump tion EU Method I Log Normal

EU Method II

Distribution-Free

California Method

μ + 3 σ

Approximate Shapiro-Francia Normality Test

### - 324 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

LEMON

Cucurbit Vegetables

The dataset used to establish MRLs for spirotetrama t in/on cucurbit vegetable, group 9 consisted of summer squash field trial data representing applica tion rates of 0.165-0.180 kg a.i./ha (100 OD formul ation) with a 1-day PHI. All but one of the 10 field tria l sample values were above the combined LOQ of 0.05 ppm. Since only one value (combined residues) was report ed below the LOQ, MLE procedures were not needed to impute censored values. Visual inspection of the lognormal probability plot provided in the spreads heet indicates that the dataset is reasonably lognormal. The result from the approximate Shapiro-Francia t est statistic confirmed that the assumption of lognorm ality should not be rejected. Using the lognormal E U Method I and the point estimate of the 99 th 

### percentile, the value is rounded to 0.30 ppm. Ther efore, 0.30 ppm is the recommended MRL level for spirotetramat in/o n cucurbit vegetable (group 9). Regulator:

Lemon 150 OD conc phi 1

Chemical:

Crop:

PHI:

App. Rate:

Submitter:

n: 10

min: 0.27

max: 0.47 median; 0.31

average: 0.34

95th Percentile 99th Percentile 99.9th Percentile

EU Method I 0.50 0.50 0.60

Normal (0.60) (0.70) (--)

0.50 0.60 0.60

(0.60) (0.80) (--)

0.80

0.60

UPLMedian 95th 3.0

0.8871 p-value > 0.05 : Do not reject lognormality assumpt ion EU Method I Log Normal

EU Method II

Distribution-Free

California Method

μ + 3 σ

Approximate Shapiro-Francia Normality Test

### - 325 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

SUMMER SQUASH

Fruiting Vegetables

The dataset used to establish an MRL for spirotetra mat in/on fruiting vegetable (group 8 ) consisted of nonbell pepper field trial data representing applicati on rates of 0.168-0.199 kg a.i./ha (100 OD formulat ion) with a 1-day PHI. All 6 field trial sample results were a bove the combined LOQ of 0.05 ppm. Since there wer e no values (combined residues) reported below the LOQ, MLE procedures were not needed to impute censored values. The spirotetramat non-bell pepper dataset w as entered into the MRL spreadsheet. Visual inspect ion of the lognormal probability plot provided in the s preadsheet indicates that the dataset is reasonably lognormal. The result from the approximate Shapiro -Francia test statistic confirmed that the assumpti on of lognormality should not be rejected. Using the log normal EU Method I and the point estimate of the 99 th 

### percentile, the value is rounded to 2.5 ppm. There fore, 2.5 ppm is the recommended MRL level for spirotetramat in/on fruiting vegetable (group 8). Regulator:

Summer Squash 100 OD phi 1

Chemical:

Crop:

PHI:

App. Rate: Submitter:

n: 11

min: 0.05

max: 0.18 median; 0.06

average: 0.09

95th Percentile 99th Percentile 99.9th Percentile

EU Method I 0.20 0.25 0.25

Normal (0.25) (0.30) (--)

0.20 0.30 0.40

(0.35) (0.60) (--)

0.30

0.25

UPLMedian 95th 0.50

0.8565 p-value > 0.05 : Do not reject lognormality assumpt ion EU Method I Log Normal

EU Method II

Distribution-Free

California Method

μ + 3 σ

Approximate Shapiro-Francia Normality Test

### - 326 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

NON-BELL PEPPER

Grapes

The dataset used to establish an MRL for spirotetra mat in/on grape consisted of field trial data representing application rates of 0.218–0.227 kg a.i./ha (100 OD formulation) with a 7-day PHI. All 24 field trial sample results were above the co mbined LOQ of 0.05 ppm. Since there were no values (combined residues) reported below the LOQ, MLE pro cedures were not needed to impute censored values. The spirotetramat grape dataset was entered into th e MRL spreadsheet. Visual inspection of the lognorm al probability plot provided in the spreadsheet indica tes that the dataset is reasonably lognormal. The result from the approximate Shapiro-Francia test statistic confirmed that the assumption of lognormality shou ld not be rejected. Using the lognormal EU Method I and t he point estimate of the 95 th 

### percentile, the value is rounded to1.3 ppm. Therefore, 1.3 ppm is the recomm ended MRL level for spirotetramat in/on small fruit vine climbing, except fuzzy kiwifruit (subgroup 13-07F). Regulator: Cayane 100 OD phi 1

Chemical:

Crop:

PHI:

App. Rate: Submitter:

n: 6

min: 0.43

max: 1.38 median; 0.56

average: 0.75

95th Percentile 99th Percentile 99.9th Percentile

EU Method I 1.4 1.7 2.0

Normal (2.5) (3.0) (--)

1.5 2.5 3.0

(4.0) (8.0) (--)

2.5

2.0

UPLMedian 95th 7.0

0.8749 p-value > 0.05 : Do not reject lognormality assumpt ion EU Method I Log Normal

EU Method II

Distribution-Free

California Method

μ + 3 σ

Approximate Shapiro-Francia Normality Test

### - 327 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

GRAPE

Hops

The dataset used to establish an MRL for spirotetra mat in/on hops consisted of field trial data representing application rates of 0.217–0.224 kg a.i./ha (100 OD formulation) with a 7-day PHI. All 6 field trial sample results were above the combined LOQ of 0.05 ppm. S ince there were no values (combined residues) reported below the LOQ, MLE procedures were not nee ded to impute censored values. The spirotetramat hop dataset was entered into the MRL spreadsheet. V isual inspection of the lognormal probability plot provided in the spreadsheet indicates that the data set is not reasonably lognormal. The result from t he approximate Shapiro-Francia test statistic confirme d that the assumption of lognormality should be rej ected. Using the CA Method and the μ + 3 σ , the value rounds to 10 ppm. Therefore, 10 ppm is the recommended MRL level for spirotetramat in/on hops (dried). Regulator: grape 150 OD phi 7

Chemical:

Crop:

PHI:

App. Rate:

Submitter:

n: 24

min: 0.11

max: 1.29 median; 0.33

average: 0.41

95th Percentile 99th Percentile 99.9th Percentile

EU Method I 0.90 1.1 1.3

Normal (1.1) (1.3) (--)

0.90 1.3 2.0

(1.3) (2.5) (--)

1.0

1.2

UPLMedian 95th 2.0

0.9601 p-value > 0.05 : Do not reject lognormality assumpt ion EU Method I Log Normal

EU Method II

Distribution-Free

California Method

μ + 3 σ

Approximate Shapiro-Francia Normality Test

### - 328 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

HOPS

Leafy Vegetables

The dataset used to establish an MRL for spirotetra mat in/on leafy vegetable, except Brassica, (group 4) consisted of spinach field trial data representing application rates of 0.170-0.183 kg a.i./ha (100 OD formulation) with a 3-day PHI. All 14 field trial sample results were above the combined LOQ of 0.05 ppm. Since there were no values (combined residues) repo rted below the LOQ, MLE procedures were not needed to impute censored values. The spirotetramat spinac h dataset was entered into the MRL spreadsheet. Vis ual inspection of the lognormal probability plotprovide d in the spreadsheet indicates that the dataset is reasonably lognormal. The result from the approxim ate Shapiro-Francia test statistic confirmed that t he assumption of lognormality should not be rejected. Using the EU Method I and the point estimate of th e 99 th 

### percentile, the value is rounded to 9.0 ppm. There fore, 9.0 ppm is the recommended MRL level for spirotetramat in/on leafy vegetable, except Brassica (group 4). Regulator: Hops 150 OD phi 7

Chemical:

Crop:

PHI:

App. Rate:

Submitter:

n: 6

min: 2.16

max: 5.82 median; 5.17

average: 4.43

95th Percentile 99th Percentile 99.9th Percentile

EU Method I 8.0 9.0 10

Normal (11) (13) (--)

9.0 12 17

(25) (45) (--)

12

10

UPLMedian 95th 60

0.7728 0.05 >= p-value > 0.01 : Reject lognormality assump tion EU Method I Log Normal

EU Method II

Distribution-Free

California Method

μ + 3 σ

Approximate Shapiro-Francia Normality Test

### - 329 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

SPINACH

Pome Fruits

The dataset used to establish an MRL for spirotetra mat in/on pome fruit, pome (group 11) consisted of pear field trial data representing application rate s of 0.430–0.447 kg a.i./ha (concentrated spray, 10 0 OD formulation) with a 7-day PHI. All 12 field trial sample results were above the combined LOQ of 0.05 ppm. Since there were no values (combined residues) repo rted below the LOQ, MLE procedures were not needed to impute censored values. The spirotetramat pear d ataset was entered into the MRL spreadsheet. Visual inspection of the lognormal probability plot provid ed in the spreadsheet indicates that the dataset is reasonably lognormal. The result from the approxim ate Shapiro-Francia test statistic confirmed that t he assumption of lognormality should not be rejected. Using the EU Method I and the point estimate of th e 99 th 

### percentile, the value is rounded to 0.70 ppm. Ther efore, 0.70 ppm is the recommended MRL level for spirotetramat in/on pome fruit, group 11. Regulator: spinach 100 OD phi 3

Chemical:

Crop:

PHI:

App. Rate: Submitter:

n: 14

min: 0.20

max: 3.36 median; 1.33

average: 1.47

95th Percentile 99th Percentile 99.9th Percentile

EU Method I 3.5 4.0 4.5

Normal (4.0) (5.0) (--)

5.0 9.0 17

(12) (30) (--)

5.0

4.5

UPLMedian 95th 10

0.8880 p-value > 0.05 : Do not reject lognormality assumpt ion EU Method I Log Normal

EU Method II

Distribution-Free

California Method

μ + 3 σ

Approximate Shapiro-Francia Normality Test

### - 330 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

PEAR

Potatoes

The dataset used to establish an MRL for spirotetra mat in/on tuberous and corm vegetable, subgroup 1C consisted of potato field trial data representing a pplication rates of ~0.179 kg a.i./ha (100 OD formu lation) with a 7-day PHI. All but two of the 32 field tria l sample values were above the combined LOQ of 0.05 ppm. Since only two values (combined residues) were repo rted below the LOQ, MLE procedures were not needed to impute censored values. The spirotetramat lemon dataset was entered into the MRL spreadsheet. Visua l inspection of the lognormal probability plot provid ed in the spreadsheet indicates that the dataset is reasonably lognormal. The result from the approxim ate Shapiro-Francia test statistic confirmed that t he assumption of lognormality should not be rejected. Using the lognormal EU Method I and the point esti mate of the 95 th 

### percentile, the value is rounded to 0.60 ppm. Ther efore, 0.60 ppm is the recommended MRL level for spirotetramat in/on tuberous and corm vegetable (subgroup 1C). Regulator:

pear 150 OD conc phi 7

Chemical:

Crop:

PHI:

App. Rate:

Submitter:

n: 12

min: 0.08

max: 0.41 median; 0.20

average: 0.20

95th Percentile 99th Percentile 99.9th Percentile

EU Method I 0.40 0.50 0.60

Normal (0.60) (0.70) (--)

0.45 0.70 1.0

(0.90) (1.5) (--)

0.70

0.60

UPLMedian 95th 1.5

0.9533 p-value > 0.05 : Do not reject lognormality assumpt ion EU Method I Log Normal

EU Method II

Distribution-Free

California Method

μ + 3 σ

Approximate Shapiro-Francia Normality Test

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

POTATOES

Stone Fruits

The dataset used to establish an MRL for spirotetra mat in/on stone fruit, group 12 consisted of cherry field trial data representing application rates of 0.264- 0.273 kg a.i./ha (concentrated spray, 100 OD formul ation) with a 7-day PHI. All 12 field trial sample result s were above the combined LOQ of 0.05 ppm. Since t here were no values (combined residues) reported below t he LOQ, MLE procedures were not needed to impute censored values. The spirotetramat cherry dataset w as entered into the MRL spreadsheet. Visual inspect ion of the lognormal probability plot provided in the s preadsheet indicates that the dataset is reasonably lognormal. The result from the approximate Shapiro -Francia test statistic confirmed that the assumpti on of lognormality should not be rejected. Using the EU Method I and the point estimate of the 99 th 

### percentile, the value rounds to 4.5 ppm. Therefore, 4.5 ppm is the recommended MRL level for spirotetramat in/on stone fruit (group 12). Regulator: potato 150 OD phi 7

Chemical:

Crop:

PHI:

App. Rate: Submitter:

n: 34

min: 0.05

max: 0.46 median; 0.12

average: 0.17

95th Percentile 99th Percentile 99.9th Percentile

EU Method I 0.40 0.50 0.60

Normal (0.45) (0.60) (--)

0.40 0.70 1.1

(0.60) (1.0) (--)

0.45

0.60

UPLMedian 95th 0.70

0.9389 p-value > 0.05 : Do not reject lognormality assumpt ion EU Method I Log Normal

EU Method II

Distribution-Free

California Method

μ + 3 σ

Approximate Shapiro-Francia Normality Test

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

CHERRIES

Tree Nuts

The dataset used to establish an MRL for spirotetra mat in/on tree nut, group 14 consisted of pecan field trial data representing application rates of 0.368-0.385 kg a.i./ha (dilute spray, 100 OD formulation) with a 7-day PHI. As 6 of 10 field trial sample results were be low the combined LOQ of 0.05 ppm, MLE procedures we re needed to impute censored values. The spirotetramat pecan dataset was entered into the MRL spreadsheet

. Visual inspection of the lognormal probability plot provided in the spreadsheet indicates that the dat aset is reasonably lognormal. The result from the approxim ate Shapiro-Francia test statistic confirmed that t he assumption of lognormality should not be rejected. Using the UPL Median 95 th 

### percentile, the value is rounded to 0.25 ppm. Therefore, 0.25 ppm is the re commended MRL level for spirotetramat in/on tree nu t (group 14). Regulator: cherry 150 OD conc 7

Chemical:

Crop:

PHI:

App. Rate:

Submitter:

n: 12

min: 0.32

max: 2.12 median; 1.32

average: 1.27

95th Percentile 99th Percentile 99.9th Percentile

EU Method I 2.5 3.0 3.0

Normal (3.0) (3.5) (--)

3.0 4.5 7.0

(6.0) (9.0) (--)

3.5

3.0

UPLMedian 95th 10

0.8921 p-value > 0.05 : Do not reject lognormality assumpt ion EU Method I Log Normal

EU Method II

Distribution-Free

California Method

μ + 3 σ

Approximate Shapiro-Francia Normality Test

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

PECAN

Strawberries (import only)

The dataset used to establish an MRL for spirotetra mat in/on strawberry consisted of field trial data representing application rates of ~0.19 kg a.i./ha (greenhouse, 100 OD formulation) with a 7-day PHI. All 8 field trial sample results were above the combined LOQ of 0.05 ppm. Since there were no values (combi ned residues) reported below the LOQ, MLE procedures we re not needed to impute censored values. The spirotetramat strawberry dataset was entered into t he MRL spreadsheet. Visual inspection of the lognor mal probability plot provided in the spreadsheet indica tes that the dataset is reasonably lognormal. The result from the approximate Shapiro-Francia test statistic confirmed that the assumption of lognormality shou ld not be rejected. Using the EU Method I and the point e stimate of the 99 th 

### percentile, the value rounds to 0.40 ppm. Therefore, 0.40 ppm is the recommended MRL lev el for spirotetramat in/on strawberries. Regulator: Pecan Nutment dilute Spray OD with MLE

Chemical:

Crop:

PHI:

App. Rate: Submitter:

n: 10

min: 0.00

max: 0.30 median; 0.03

average: 0.10

95th Percentile 99th Percentile 99.9th Percentile

EU Method I 0.30 0.40 0.50

Normal (0.45) (0.60) (--)

0.60 1.6 6.0

(4.0) (25) (--)

0.40

0.50

UPLMedian 95th 0.25

0.9419 p-value > 0.05 : Do not reject lognormality assumpt ion EU Method I Log Normal

EU Method II

Distribution-Free

California Method

μ + 3 σ

Approximate Shapiro-Francia Normality Test

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

STRAWBERRY (EU)

Dry Bulb Onions (import only)

The dataset used to establish an MRL for spirotetra mat in/on dry bulb onion, subgroup 3-07A consisted of field trial data representing application rates of ~0.29 kg a.i./ha (Northern EU, 100 OD formulation) with a 7- day PHI. All 8 field trial sample results were abo ve the combined LOQ of 0.05 ppm. Since there were no values (combined residues) reported below the LOQ, MLE procedures were not needed to impute censored values. The spirotetramat strawberry dataset was en tered into the MRL spreadsheet. Visual inspection o f the lognormal probability plot provided in the spreadsh eet indicates that the dataset is reasonably lognor mal. The result from the approximate Shapiro-Francia tes t statistic confirmed that the assumption of lognor mality should not be rejected. Using the EU Method I and the point estimate of the 99 th 

### percentile, the value rounds to 0.30 ppm. Therefore, 0.30 ppm is the recommended MRL level for spirotetramat in/on dry bulb onions. Regulator: EU

Chemical: SPA Crop: Strawberry Greenhouse

PHI: 7

App. Rate: 192 g as/ha

Submitter:

n: 8

min: 0.21

max: 0.33 median; 0.28

average: 0.27

95th Percentile 99th Percentile 99.9th Percentile

EU Method I 0.35 0.40 0.40

Normal (0.40) (0.45) (--)

0.35 0.40 0.45

(0.45) (0.60) (--)

0.70

0.40

UPLMedian 95th 3.0

0.9451 p-value > 0.05 : Do not reject lognormality assumpt ion EU Method I Log Normal

EU Method II

Distribution-Free

California Method

μ + 3 σ

Approximate Shapiro-Francia Normality Test

### - 335 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

DRY BULB ONIONS

Regulator: EU

Chemical: Spirotetramat

Crop: Onion Northern EU

PHI: 7

App. Rate: 288 g ai/ha of 100 or 150OD

Submitter:

n: 8

min: 0.05

max: 0.20 median; 0.10

average: 0.11

95th Percentile 99th Percentile 99.9th Percentile

EU Method I 0.20 0.25 0.30

Normal (0.30) (0.35) (--)

0.25 0.30 0.40

(0.40) (0.70) (--)

0.30

0.30

UPLMedian 95th 1.0

0.9558 p-value > 0.05 : Do not reject lognormality assumpt ion EU Method I Log Normal

EU Method II

Distribution-Free

California Method

μ + 3 σ

Approximate Shapiro-Francia Normality Test

### - 336 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Annex III: Import tolerances (evaluation document o f UK):

MRL PROPOSALS FOR SPIROTETRAMAT [NEW ACTIVE SUBSTAN CE; OECD WORK SHARING PROJECT]

EU RAPPORTEUR MEMBER STATE: AUSTRIA

February 2008

Introduction

This MRL proposal results from an OECD work sharing project for the new active substance spirotetremat

. A range of uses are proposed both in the EU and in the USA, Canada and Mexico (NAFTA countries). Different components of the data evaluation have be en performed by AGES (Austria), EPA (USA), PMRA (Canada) and PSD (UK). This document provides an o verview of GAPs and residues data in support of EU MRLs to be established in Regulation 396/2005. The assessment considers data and GAPs for both EU and NAFTA and proposes MRLs on the basis of the most cr itical data and GAP for each use, subject to acceptable consumer risk assessment.

Acceptable Daily Intake (ADI) for spirotetramat Set by US EPA and AGES (2007) ADI 0.05 mg/kg bw/day NOAEL 5 mg/kg bw/day Study type 1 year dog study.

Set by PMRA, Canada (2007) ADI 0.03 mg/kg bw/day NOAEL 1 mg/kg bw/day Study type Teratogenicity rabbit study.

Acute Reference Dose (ARfD) for spirotetramat Set by US EPA, PMRA, Canada (2007) and AGES (2008) ARfD 1 mg/kg bw/day NOAEL 100 mg/kg bw/day Study type acute neurotox rat study

Residue definition for spirotetramat The residue definition for plants for monitoring an d risk assessment is ‘Sum of spirotetramat, BYI0833 0-enol, BYI08330-ketohydroxy, BYI08330-monohydroxy, and BYI 08330 enol-glucoside, expressed as spirotetramat’.

Limits of determination 0.02 mg/kg for plants (total residue) 0.01-0.05 mg/kg for products of animal origin

Trial selection For all trials, the residue value corresponding to the notified GAP was used, unless for decline trial s, the residue value was higher at a longer PHI. For NAFT A trials, several plots were sampled from the same sites

### - 337 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

each year, with replicate samples from each plot re ported. Plots on each site were also sprayed with different formulations. In all cases, only a singl e residue value from each site for each year was us ed for MRL calculations. The selected value was the highe st single replicate value for that site.

GAP tables are given in Appendix 1 and details of a ll trials are given in Appendix 2.

ASSESSMENT OF CONSUMER RISK

Both acute and chronic intake resulting from the pr oposed uses have been calculated using the EFSA consumer risk assessment model. A first tier asses sment using proposed MRL values indicates a maximum of 68% of the ARfD (Kale) and a total chronic intak e of 77% of the ADI (German child). All proposed M RLs are therefore regarded as acceptable for consumers and no further refinement of the risk assessment is required.- 338 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008CommodityCodex EUProposedSTMR(mg/kg)Remarks Comments by RMS Austria:1. FRUIT FRESH OR FROZEN;NUTS(i) Citrus fruit1 0.34 GAP in EU-S: 2x0.096 kg as./ha, 14 day PHIGAP NAFTA:2x0.180 kg as./ha, 1 day PHINAFTA data critical. Oranges and lemon combinedfor group tolerance. Lemon data appear to be higherthan oranges and therefore suitable alternative tomandarin for group tolerance.Rmax = 0.52Rber = 0.78Proposal by Canada: 0.6 mg/kg;difference between the two proposalsbased on different calculation-modelsand/or MRL-classes.Grapefruit RESIDUE TRIALSEUNo dataNAFTA0.26; <0.25; <0.25; <0.25; 0.35; <0.25Oranges RESIDUE TRIALSEU-S0.06; 0.06; 0.06; 0.07; 0.08; 0.11; 0.12; 0.23NAFTA0.42; <0.25; 0.38; 0.34; 0.43; <0.25; 0.32; 0.34; <0.25Lemons RESIDUE TRIALSNAFTA0.28; 0.36; 0.47; 0.33; 0.34Limes- 339 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Mandarins RESIDUE TRIALSEU-S0.14; 0.15; 0.17; 0.19; 0.21; 0.23; 0.23; 0.27; 0.33NAFTANo dataOthers1(ii) Tree nuts (shelled orunshelled)0.5 0.07 No GAP in EUGAP NAFTA: 2x0.19 kg as/ha, 7 days PHI.Almonds and pecans combined for group toleranceRmax = 0.34Rber = 0.29Proposal by Canada: 0.25 mg/kg;difference between the two proposalsbased on different calculation-modelsand/or MRL-classes.Almond hulls 9 mg/kg (proposalCanada): not considered because nofood item in EU.Almonds RESIDUE TRIALSNAFTA<0.05; 0.14; 0.08; 0.06; 0.14 mg/kgBrazil nutsCashew nutsChestnutsCoconutsHazelnutsMacadamiaPecans RESIDUE TRIALSNAFTA0.06; <0.05; <0.05; 0.16; 0.30 mg/kgPine nutsPistachiosWalnutsOthers2- 340 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008(iii) Pome fruit0.5 0.18 GAP in EU-N and S: 2x0.072 kg as /ha, 21day PHIGAP NAFTA: 3x0.150 kg as/ha, 7 days PHINAFTA data critical. Apples and pears combined forgroup toleranceRmax = 0.45Rber = 0.501 mg/kg might be moreappropriate; covering Canada’sproposal of 0.7 mg/kg).Apples RESIDUE TRIALSEU-S (critical data)0.05; 0.10; 0.10; 0.13; 0.14; 0.19NAFTA0.06; 0.17; 0.14; 0.13; 0.08; 0.07; 0.38; 0.37; 0.34; 0.18;0.18; 0.12Pears RESIDUE TRIALSEU-S critical data0.05; 0.07; 0.07; 0.14; 0.15; 0.25NAFTA0.12; 0.37; 0.21; 0.22; 0.22; 0.11;QuincesMedlarLoquatOthers3(iv) Stone fruitGAP in EU-N and S: 2x0.072 kg as /ha, 21 day PHIGAP NAFTA: 2x0.140 kg as/ha, 7 days PHIApricots 2 0.70 RESIDUE TRIALSEU-S critical data0.27; 0.28; 0.29; 0.68; 0.69Extrapolation from NAFTA peach dataExtrapolation from NAFTA peachdataCanada’s proposal: 4.5 mg/kg (grouptolerance stone fruits – based oncherry data?)- 341 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Cherries 5 1.63 RESIDUE TRIALSEU-NSweet cherry critical data: 0.52; 0.58; 0.83; 0.94;EU-SSweet cherry critical data: 0.63; 0.68; 0.72; 1.05Data can be combined, no significant difference betweenN and SNAFTA2.13; 1.63; 2.12; 0.75; 1.63; 1.63NAFTA data critical.Rmax = 3.51Rber = 4.25Canada’s proposal: 4.5 mg/kg (grouptolerance stone fruits); differencebetween the two proposals based ondifferent calculation-models and/orMRL-classes.Peaches 2 0.70 RESIDUE TRIALSEU-S critical data0.12; 0.17; 0.31; 0.35NAFTA0.70; 0.56; 0.53; 0.82; 0.69; 1.23; 0.69; 0.77; 0.77NAFTA data critical.Rmax = 1.37Rber = 1.59Canada’s proposal: 4.5 mg/kg (grouptolerance stone fruits – based oncherry data?)- 342 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Plums 2 0.36 RESIDUE TRIALSEU-N0.12; 0.15; 0.19; 0.35; 0.42; 0.51; 0.58; 0.83NAFTA0.84; 0.37; 0.23; 0.35; 0.11; 0.57NAFTA data critical. (Major in N EU, but only 6 trials –ACCEPTABLE IF RISK LOW?)Rmax = 1.38Rber = 1.28Based on 6 trials only (mafor crop inN-EU).. Proposal by Canada: 4.5mg/kg; (group tolerance stone fruits –based on cherry data?)Others4 0.02* No GAPThe LOQ of the analytical method is0.05 mg/kg for the total residue.(v) Berries & small fruit(a) Table and wine grapes2 0.36 GAP in EU- S: 2x0.096 kg as /ha, 14 day PHIGAP NAFTA: 2x0.110 kg as /ha, 7 day PHIRESIDUE TRIALS (combined table and wine, no apparentdifference)EU-S0.48; 0.18; 0.26; 0.64; 0.28; 0.22; 0.17; 0.57; 0.20; 0.35NAFTA0.32; 0.79; 0.24; 0.29; 0.26; 0.11; 0.48; 0.50; 0.34; 0.47;1.29; 0.38NAFTA data critical.Rmax = 1.31Rber = 0.99Proposal by Canada: 1.3 mg/kg;difference between the two proposalsbased on different calculation-modelsand/or MRL-classes.Table grapesWine grapes- 343 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008(b) Strawberries1 0.28 GAP in EU-N, S and glasshouse: 2x0.096 kg as /ha, 3day PHIRESIDUE TRIALSEU-G0.28; 0.21; 0.24; 0.33; 0.29; 0.23; 0.28; 0.30EU-N0.18; 0.16; 0.26; 0.21EU-S0.14; 0.15; 0.14; 0.11EU Glasshouse data critical.Rmax = 0.40Rber = 0.60No import tolerance, as no useintended within NAFTA.(c) Cane fruit0.02* No GAPThe LOQ of the analytical method is0.05 mg/kg for the total residue.BlackberriesDewberriesRaspberriesOthers5(d) Other small fruit & berries0.02* No GAPThe LOQ of the analytical method is0.05 mg/kg for the total residue.BlueberriesCranberriesCurrants (red, black andwhite)GooseberriesRose hipsMulberries- 344 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Azarole (mediteraneanmedlar)ElderberriesOthers6(vi) Miscellaneous fruit0.02* No GAPThe LOQ of the analytical method is0.05 mg/kg for the total residue.(a) Edible peelDatesFigsTable olivesKumquatsCarambolaPersimmonJambolan (java plum)Others7(b) Inedible peel, smallKiwiLychee (Litchi)Passion fruitPrickly pear (cactus fruit)Star appleAmerican persimmon(Virginia kaki)Others8(c) Inedible peel, largeAvocadosBananasMangoesPapaya- 345 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008PomegranateCherimoyaGuavaPineapplesBread fruitDurianSoursop (guanabana)Others92. VEGETABLES FRESH ORFROZEN(i) Root and tuber vegetables(a) Potatoes0.5 0.12 No GAP in EUGAP NAFTA: 0.18 kg as/ha, 7 days PHI.RESIDUE TRIALSNAFTA0.41; 0.19; 0.25; 0.31; 0.17; 0.07; 0.45; 0.08; 0.10; <0.05;0.08; 0.07; 0.12; 0.17; 0.12; 0.08Rmax = 0.48Rber = 0.47Proposal doesn’t cover CanadasMRL of 0.6 mg/kg:difference between the two proposalsbased on different calculation-modelsand/or MRL-classes.(b) Tropical root and tubervegetables0.02* No GAPThe LOQ of the analytical method is0.05 mg/kg for the total residue.CassavaSweet potatoesYamsArrowrootOthers10(c) Other root and tubervegetables except sugar beet0.02* No GAPThe LOQ of the analytical method is0.05 mg/kg for the total residue.- 346 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008BeetrootCarrotsCeleriacHorseradishJerusalem artichokesParsnipsParsley rootRadishesSalsifySwedesTurnipsOthers11(ii) Bulb vegetablesGarlicOnions 0.5 0.11 GAP in EU-N: 4x0.072 kg as/ha, 7 day PHIRESIDUE TRIALSEU-N0.20; 0.10; 0.11; 0.11; 0.16; <0.05; 0.08; 0.09EU-S0.07; 0.12; 0.10; 0.17; 0.08; 0.09; 0.14; <0.05EU-N data critical.Rmax = 0.26Rber = 0.30No NAFTA GAP, therefore no importtolerance.ShallotsSpring onionsOthers12 0.02* No GAPThe LOQ of the analytical method is0.05 mg/kg for the total residue.- 347 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008(iii) Fruiting vegetables(a) SolanaceaTomatoes 2 0.44 GAP in EU-S and glasshouse:4x0.072 kg as /ha, 3 dayPHIGAP NAFTA: 2x0.090 kg as /ha, 1 day PHIRESIDUE TRIALSEU-G0.44; 0.44; 0.74; 0.68; 0.51; 0.29; 0.34; 0.22EU-S0.19; 0.14; 0.12; 0.21NAFTA0.12; 0.11; 0.22; 0.08; 0.10; 0.23; 0.22; 0.14; 0.17; 0.11;0.18; 0.14EU-G data critical.Rmax = 1.04Rber = 1.28No NAFTA GAP, therefore no importtolerance.- 348 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Peppers 2 0.48 GAP in EU-S and glasshouse:4x0.072 kg as /ha, 3 dayPHIGAP NAFTA: 2x0.090 kg as /ha, 1 day PHIRESIDUE TRIALSEU-G0.57; 0.58; 0.43; 0.35; 0.55; 0.48; 0.27; 0.54; 0.48; 0.57;0.31; 0.29EU-S0.82; 0.27; 0.21; 0.35; 0.14; 0.17; 0.11; 0.17NAFTASweet pepper: 0.17; 0.28; 0.57; 0.36; 0.68; 0.32Chilli pepper: 1.38; 0.58; 0.48NAFTA data critical (combined sweet and chillipepper).Rmax = 1.62Rber = 1.26Corresponding to MRL-proposalbased on critical EU-GAP(glasshouse).Aubergines (egg plants) 2 0.44 GAP in EU-Sand glasshouse: 4x0.072 kg as /ha, 3 dayPHIExtrapolated from tomatoOkra, lady’s fingersOthers13 0.02* No GAPThe LOQ of the analytical method is0.05 mg/kg for the total residue.(b) Cucurbits - edible peel- 349 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Cucumbers 0.2 0.06 GAP in EU-S and glasshouse: 4x0.072 kg as /ha, 3 dayPHIGAP NAFTA: 2x0.090 kg as /ha, 1 day PHIRESIDUE TRIALSEU-G0.08; 0.06; 0.07; 0.07; 0.08; <0.05; 0.06; 0.06EU-S0.06; <0.05; 0.06; 0.06; <0.05; <0.05; 0.12NAFTA<0.05; 0.07; <0.05; <0.05; 0.06; 0.08EU data critical (G and S data can be combined, nosignificant difference).Rmax = 0.11Rber = 0.14Corresponding to MRL-proposalbased on critical EU-GAP(glasshouse);Canada’s proposal: 0.3 mg/kg,difference based on differentcalculation modelsGherkinsCourgettes 0.2 0.06 GAP in EU-S and glasshouse: 4x0.072 kg as /ha, 3 dayPHIExtrapolated from cucumberOthers14 0.02* No GAPThe LOQ of the analytical method is0.05 mg/kg for the total residue.(c) Cucurbits-inedible peel0.3 0.06 GAP in EU-S and glasshouse: 4x0.072 kg as/ha, 3 dayPHIGAP NAFTA: 2x0.090 kg as /ha, 1 day PHINAFTA data critical. Melons and squashes combinedfor group tolerance.Rmax = 0.11Rber = 0.14Corresponds to proposal by Canada.- 350 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Melons RESIDUE TRIALSEU-G<0.05; <0.05; 0.06; <0.05; <0.05; <0.05; 0.06; <0.05EU-S0.08; <0.05; 0.09; <0.05; 0.08; 0.06; 0.06; <0.05;<0.05NAFTA0.06; <0.05; 0.13; 0.08; 0.06; <0.05Pumpkins RESIDUE TRIALSNAFTA0.18; 0.05; 0.08; 0.06; 0.11WatermelonsOthers15(d) Sweet corn0.02* No GAPThe LOQ of the analytical method is0.05 mg/kg for the total residue.(e) Other fruiting vegetables(iv) Brassica vegetablesGAP in EU-N and S: 2x0.072 kg as /ha, 3 day PHIGAP NAFTA: 2x0.088 kg as /ha, 1 day PHI(a) Flowering brassica2 0.50 RESIDUE TRIALS (Data)EU-N0.58; 0.43; 0.24; 0.38; 0.11; 0.22; 0.31; 0.37EU-S0.32; 0.26; 0.20; 0.13NAFTA0.87; 0.84; 0.55; 0.18; 0.35; 0.29; 0.54; 0.45NAFTA data critical (combined for broccoli andcauliflower).Rmax = 1.30Rber = 1.54Proposal by Canada: 2.5 mg/kg;difference between the two proposalsbased on different calculation-modelsand/or MRL-classes.Broccoli- 351 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008CauliflowerOthers16(b) Head brassicaBrussels sprouts 0.3 0.11 RESIDUE TRIALSEU-N0.11; 0.09; 0.13; 0.22; 0.09; 0.09; 0.14; 0.11Rmax = 0.26Rber = 0.28No NAFTA GAP, therefore no importtolerance.Head cabbage 2 0.24 RESIDUE TRIALSEU-N0.10; 0.10; 0.09; 0.07; 0.13; 0.19; 0.08; 0.26; 0.09; 0.15EU-S0.23; 0.11; 0.07; 0.07NAFTA0.07; 0.92; 0.06; 0.65; 0.24; 0.51; 0.19NAFTA data criticalRmax = 1.30Rber = 1.54Proposal by Canada: 2.5 mg/kg;difference between the two proposalsbased on different calculation-modelsand/or MRL-classes.Others17 0.02* No GAPThe LOQ of the analytical method is0.05 mg/kg for the total residue.- 352 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008(c) Leafy brassica10 3.70 RESIDUE TRIALSEU-N0.62; 0.77; 0.24; 0.30EU-S0.56; 0.63; 0.31; 0.21NAFTA1.73; 5.49; 4.02; 5.60; 0.87; 0.86; 2.01; 3.38; 4.46; 4.29NAFTA data criticalRmax = 8.49Rber = 9.44Proposal by Canada: 8.0 mg/kg;difference between the two proposalsbased on different calculation-modelsand/or MRL-classes.Chinese cabbageKaleOthers18(d) Kohlrabi5 0.47 RESIDUE TRIALSEU-N1.43; 0.67; 0.27; 0.16Rmax = 3.59Rber = 2.48Wrong residue data. The correct dataare :0.152, 0.232, 0.554, 0.670Rmax = 1.648Rber = 1.282HR 0.670 mg/kgSTMR 0.393mg/kgMRL: 2 mg/kg(v) Leaf vegetables & freshherbs(a) Lettuce and other saladplants including BrassicaceaLamb's lettuce- 353 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Lettuce 5 1.24 GAP in EU-N, S and glasshouse: 2x0.072 kg as /ha, 7day PHIRESIDUE TRIALSEU-G1.06; 0.39; 1.76; 0.37; 1.84; 1.41; 0.16; 2.33;Rmax = 3.72Rber = 3.64Intended for use in NAFTA, but noresidue trials submitted.Scarole (broad-leaf endive)CressLand cressRocket, RucolaRed mustardLeaves and sprouts ofBrassica sppOthers19 0.02* No GAPThe LOQ of the analytical method is0.05 mg/kg for the total residue.(b) Spinach & similar (leaves)0.02* No GAPThe LOQ of the analytical method is0.05 mg/kg for the total residue.SpinachPurslaneBeet leaves (chard)Others20(c) Vine leaves (grape leaves)(d) Water cress0.02* No GAPThe LOQ of the analytical method is0.05 mg/kg for the total residue.(e) Witloof0.02* No GAPThe LOQ of the analytical method is0.05 mg/kg for the total residue.- 354 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008(f) Herbs0.02* No GAPThe LOQ of the analytical method is0.05 mg/kg for the total residue.ChervilChivesCelery leavesParsleySageRosemaryThymeBasilBay leaves (laurel)TarragonOthers21(vi) Legume vegetables (fresh)Beans (with pods) 2 0.35 GAP in EU-glasshouse: 4x0.072 kg as /ha, 14 day PHIRESIDUE TRIALSEU-G0.30; 0.12; 0.57; 0.56; 0.08; 0.21; 0.62; 0.40Rmax = 1.03Rber = 1.14Beans (without pods)Peas (with pods)Peas (without pods)LentilsOthers22 0.02* No GAPThe LOQ of the analytical method is0.05 mg/kg for the total residue.- 355 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008(vii) Stem vegetables (fresh)0.02* No GAPThe LOQ of the analytical method is0.05 mg/kg for the total residue.AsparagusCardoonsCeleryFennelGlobe artichokesLeekRhubarbBamboo shootsPalm heartsOthers23(viii) Fungi0.02* No GAPThe LOQ of the analytical method is0.05 mg/kg for the total residue.CultivatedWildOthers24(ix). Sea weeds3. PULSES, DRY0.02* No GAPThe LOQ of the analytical method is0.05 mg/kg for the total residue.BeansLentilsPeasLupinsOthers254. OILSEEDS AND OILFRUITS0.05* No GAP(i) OilseedsLinseedPeanuts- 356 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Poppy seedSesame seedSunflower seedRape seedSoya beanMustard seedCotton seedPumpkin seedsSafflowerBorageGold of pleasureHempseedCastor beanOthers26(ii) OilfruitsOlives for oil productionPalm nuts (palmoil kernels)PalmfruitKapokOthers275. CEREALS0.02* No GAPThe LOQ of the analytical method is0.05 mg/kg for the total residue.BarleyBuckwheatMaizeMilletOatsRice- 357 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008RyeSorghumWheatOthers286. TEA, COFFEE, HERBALINFUSIONS AND COCOA0.05* No GAP(i) Tea (dried leaves andstalks, fermented or otherwiseof Camellia sinensis)(ii) Coffee beans(iii) Herbal infusions (dried)(a) FlowersCamomille flowersHybiscus flowersRose petalsJasmine flowersLime (linden)Others29(b) LeavesStrawberry leavesRooibos leavesMatéOthers30(c) RootsValerian rootGinseng rootOthers31(d) Other herbal infusions(iv) Cocoa (fermented beans)- 358 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008(v) Carob (st johns bread)7. HOPS (dried) , including hoppellets and unconcentratedpowder20 5.81 GAP EU-N: 0.35 kg as/ha, 14 days PHIGAP NAFTA: 0.224 kg as/ha, 7 days PHI.RESIDUE TRIALSEU-N: 1.64; 1.82; 4.02; 4.34NAFTA: 5.82; 5.81; 4.51NAFTA data critical. (only 3 trials – ACCEPTABLE IFRISK LOW?)Rmax = 11.15Rber = n/aBased on 3 trials only. Proposal byCanada: 10.0 mg/kg; differencebetween the two proposals based ondifferent calculation-models and/orMRL-classes.8. SPICES(i) SeedsAniseBlack carawayCelery seedCoriander seedCumin seedDill seedFennel seedFenugreekNutmegOthers32(ii) Fruits and berriesAllspiceAnise pepper (Japan pepper)CarawayCardamomJuniper berries- 359 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Pepper, black and whiteVanilla podsTamarindOthers33(iii) BarkCinnamonOthers34(iv) Roots or rhizomeLiquoriceGingerTurmeric (Curcuma)Horse-radishOthers35(v) BudsClovesCapersOthers36(vi) Flower stigmaSaffronOthers37(vii) ArilMaceOthers389. SUGAR PLANTSSugar beet (root)Sugar caneChicory rootsOthers39- 360 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 200810. PRODUCTS OF ANIMALORIGIN-TERRESTRIALANIMALS0.02* Not required0.02 mg/kg was proposed by Canadaas MRL at LOQ-Level for fat, kidney,muscle and liver. The LOQ ofBYI08330-enol calculated andexpressed as BYI08330 parentequivalents is 0.01 mg/kg; parentspirotetramat was not found in anylivestock tissue. Please, see pointB.7.8 for MRL proposal relevant forEU.(i) Meat, preparations of meat,offals, blood, animal fats freshchilled or frozen, salted, inbrine, dried or smoked orprocessed as flours or meals;other processed products suchas sausages and foodpreparations based on these(a) SwineMeat1Fat free of lean meatLiver1Kidney1Edible offal1Others40(b) BovineMeat2Fat1Liver2Kidney2Edible offal2- 361 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Others41(c) SheepMeat3Fat2Liver3Kidney3Edible offal3Others42(d) GoatMeat4Fat3Liver4Kidney4Edible offal4Others43(e) Horses, asses, mules orhinniesMeat5Fat4Liver5Kidney5Edible offal5Others44(f) Poultry -chicken, geese,duck, turkey and Guinea fowl-,ostrich, pigeonMeat6Fat5Liver6- 362 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008Kidney6Edible offal6Others45(g) Other farm animalsMeat7Fat6Liver7Kidney7Edible offal7Others46(ii) Milk and cream, notconcentrated, nor containingadded sugar or sweeteningmatter, butter and other fatsderived from milk, cheese andcurdCattleSheepGoatHorseOthers47(iii) Birds’ eggs, freshpreserved or cooked; Shelledeggs and egg yolks fresh,dried, cooked by steaming orboiling in water, moulded,frozen or otherwise preservedwhether or not containingadded sugar or sweeteningmatter- 363 -Spirotetramat – Volume 3, Annex B.7 Residue dataApril 2008ChickenDuckGooseQuailOthers48(iv) Honey(v) Amphibians and reptiles(vi) Snails(vii) Other terrestrial animalproducts*Limit of determination.

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

APPENDIX 2 - RESIDUES DATA SUMMARY FROM SUPERVISED TRIALS (SUMMARY) (NAFTA only, as EU residue data are listed yet in A nnex I.)

CITRUS Residues (ppm) Study Trial No. Trial SubID Country Year RAC PHI (days) BYI

08330 BYI

08330 cis-enol BYI 08330

cis-ketohydroxy BYI 08330

monohydroxy BYI 08330

enolglucoside Total

BYI08330 *

Orange

fruit 0

0 1 1 1 1 1 7 7 10 10 15 15 0.203

0.199 0.127 0.111 0.104 0.095 0.090 0.097 0.095 0.081 0.073 0.081 0.087 0.077

0.069 0.142 0.137 0.148 0.063 0.075 0.075 0.061 0.061 0.059 0.059 0.063 <0.050

<0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050

<0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050

<0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 0.430

0.418 0.419 0.398 0.402 0.308 0.315 0.322 0.306 0.292 0.282 0.290 0.300

fruit without peel 1

1 1 <0.050

<0.050 <0.050 <0.050

<0.050 <0.050 <0.050

<0.050 <0.050 <0.050

<0.050 <0.050 <0.050

<0.050 <0.050 0.250

0.250 0.250 RAFNY008 FN161-05D FN161-05D-A USA Clermont, Florida 2005

peel 1 1 1 0.241

0.218 0.222 0.351

0.323 0.308 0.106

0.100 0.092 <0.050

<0.050 <0.050 0.057

0.050 0.054 0.805

0.741 0.726

RAFNY008 FN161-05D FN161-05D-B USA Clermont, Florida 2005 Orange

fruit 1

1 0.057

0.055 0.078

0.079 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.285

0.284

RAFNY008 FN162-05H FN162-05H-A USA Haines City, Florida 2005 Orange

fruit 1

1 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.250

0.250

RAFNY008 FN162-05H FN162-05H-B USA Haines City, Florida 2005 Orange

fruit 1

1 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.250

0.250

RAFNY008 FN163-05H FN163-05H-A USA Oviedo, Florida 2005 Orange

fruit 1

1 0.182

0.131 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.382

0.331

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues (ppm) Study Trial No. Trial SubID Country Year RAC PHI (days) BYI

08330 BYI

08330 cis-enol BYI 08330

cis-ketohydroxy BYI 08330

monohydroxy BYI 08330

enolglucoside Total

BYI08330 *

RAFNY008 FN163-05H FN163-05H-B USA Oviedo, Florida 2005 Orange

fruit 1

1 0.094

0.109 <0.050

0.051 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.294

0.310

RAFNY008 FN164-05H FN164-05H-A USA Oviedo, Florida 2005 Orange

fruit 1

1 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.250

0.250

RAFNY008 FN164-05H FN164-05H-B USA Oviedo, Florida 2005 Orange

fruit 1

1 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.250

0.250

RAFNY008 FN165-05H FN165-05H-A USA Oviedo, Florida 2005 Orange

fruit 1

1 0.133

0.151 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.333

0.351

RAFNY008 FN165-05H FN165-05H-B USA Oviedo, Florida 2005 Orange

fruit 1

1 0.103

0.094 0.072

0.076 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.325

0.320

RAFNY008 FN166-05H FN166-05H-A USA Mt Dora, Florida 2005 Orange

fruit 1

1 0.117

0.138 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.317

0.338

RAFNY008 FN166-05H FN166-05H-B USA Mt Dora, Florida 2005 Orange

fruit 1

1 0.090

0.088 <0.050

0.052 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.290

0.290

RAFNY008 FN167-05H FN167-05H-A USA Vero Beach, Florida 2005 Orange

fruit 1

1 0.207

0.194 <0.050

<0.050 0.076

0.077 <0.050

<0.050 <0.050

<0.050 0.433

0.421

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues (ppm) Study Trial No. Trial SubID Country Year RAC PHI (days) BYI

08330 BYI

08330 cis-enol BYI 08330

cis-ketohydroxy BYI 08330

monohydroxy BYI 08330

enolglucoside Total

BYI08330 *

RAFNY008 FN167-05H FN167-05H-B USA Vero Beach, Florida 2005 Orange

fruit 1

1 0.119

0.105 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.319

0.305

RAFNY008 FN168-05H FN168-05H-A USA Vero Beach, Florida 2005 Orange

fruit 1

1 0.175

0.174 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.375

0.374

RAFNY008 FN168-05H FN168-05H-B USA Vero Beach, Florida 2005 Orange

fruit 1

1 0.135

0.156 0.062

0.069 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.347

0.375

RAFNY008 FN169-05H FN169-05H-A USA Raymondville, Texas 2005 Orange

fruit 1

1 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.250

0.250

RAFNY008 FN169-05H FN169-05H-B USA Raymondville, Texas 2005 Orange

fruit 1

1 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.250

0.250

RAFNY008 FN170-05H FN170-05H-A USA Fresno, California 2005 Orange

fruit 1

1 0.083

0.119 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.283

0.319

RAFNY008 FN170-05H FN170-05H-B USA Fresno, California 2005 Orange

fruit 1

1 <0.050

0.058 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.250

0.258

RAFNY008 FN171-05H FN171-05H-A USA Bakersfield, California 2006 Orange

fruit 1

1 0.119

0.136 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.319

0.336

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues (ppm) Study Trial No. Trial SubID Country Year RAC PHI (days) BYI

08330 BYI

08330 cis-enol BYI 08330

cis-ketohydroxy BYI 08330

monohydroxy BYI 08330

enolglucoside Total

BYI08330 *

RAFNY008 FN171-05H FN171-05H-B USA Bakersfield, California 2006 Orange

fruit 1

1 0.098

0.093 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.298

0.293

RAFNY008 FN172-05H FN172-05H-A USA Porterville, California 2005 Orange

fruit 1

1 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.250

0.250

RAFNY008 FN172-05H FN172-05H-B USA Porterville, California 2005 Orange

fruit 1

1 <0.050

0.053 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 <0.050

<0.050 0.250

0.253

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Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

TREE NUTS

Residues (ppm) Study Trial No. Trial SubID Country Year Crop

Portion analysed PHI

(days) BYI

08330 BYI

08330cisenol BYI 08330

ketohydroxy BYI 08330

monohydroxy BYI

08330enolglucoside Total

BYI08330 calc. *

Almond (Nut without shell) 0

0 6 6 10 10 13 13 21 21 0.014

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.020 0.025 0.019 0.022 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 0.054

0.05 0.05 0.05 0.05 0.05 0.06 0.065 0.059 0.062 RAFNY010 FN202-05H FN202-05D-A USA Fresno, California 2005

Almond

(hull) 0

0 6 6 10 10 13 13 21 21 1.082

1.394 1.528 3.336 2.737 2.078 1.912 1.480 1.664 2.255 <0.20

<0.20 <0.20 0.579 0.240 <0.20 <0.20 <0.20 <0.20 0.201 <0.20

<0.20 <0.20 0.429 <0.20 <0.20 <0.20 <0.20 <0.20 <0.20 <0.20

<0.20 <0.20 0.407 <0.20 <0.20 <0.20 <0.20 <0.20 <0.20 <0.20

<0.20 <0.20 <0.20 <0.20 <0.20 <0.20 <0.20 <0.20 <0.20 1.882

2.194 2.328 4.951 3.577 2.878 2.712 2.28 2.464 3.056 Almond (Nut without shell) 6

6 13 13 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 0.079 0.067 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 0.024 0.022 <0.010

<0.010 0.012 <0.010 0.05

0.05 0.135 0.119 RAFNY010 FN202-05H FN202-05D-B USA Fresno, California 2005 Almond

(hull) 6

6 13 13 3.075

1.540 3.561 3.173 0.546

<0.20 0.634 0.538 0.436

<0.20 0.517 0.440 0.312

<0.20 0.332 0.474 <0.20

<0.20 <0.20 <0.20 4.569

2.34 5.244 4.825 Almond (Nut without shell) 7

7 0.036

0.026 0.058

0.045 <0.010

<0.010 0.016

0.014 0.018

<0.010 0.138

0.105 RAFNY010 FN203-05H FN203-05H-A USA Kerman, California 2005 Almond

(hull) 7

7 2.885

2.950 0.314

0.347 <0.20

<0.20 0.492

0.476 <0.20

<0.20 4.091

4.173

Almond (Nut without shell) 7

7 0.032

0.025 0.059

0.047 <0.010

<0.010 0.014

0.012 0.012

<0.010 0.127

0.104 RAFNY010 FN203-05H FN203-05H-B USA Kerman, California 2005 Almond

(hull) 7

7 1.079

1.923 0.295

0.441 <0.20

0.230 0.528

0.676 0.281

0.372 2.383

3.642

Almond (Nut without shell) 7

7 0.025

0.024 0.029

0.021 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 0.084

0.075 RAFNY010 FN204-05H FN204-05H-A USA Glenn, California 2005 Almond

(hull) 7

7 0.603

0.461 <0.20

<0.20 <0.20

<0.20 <0.20

<0.20 <0.20

<0.20 1.403

1.261

### - 369 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues (ppm) Study Trial No. Trial SubID Country Year Crop

Portion analysed PHI

(days) BYI

08330 BYI

08330cisenol BYI 08330

ketohydroxy BYI 08330

monohydroxy BYI

08330enolglucoside Total

BYI08330 calc. *

Almond (Nut without shell) 7

7 0.025

0.029 0.028

0.021 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 0.083

0.08 RAFNY010 FN204-05H FN204-05H-B USA Glenn, California 2005 Almond

(hull) 7

7 0.614

0.634 <0.20

<0.20 <0.20

<0.20 <0.20

<0.20 <0.20

<0.20 1.414

1.434

Almond (Nut without shell) 7

7 0.017

0.021 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 0.057

0.061 RAFNY010 FN205-05H FN205-05H-A USA Dinuba, California 2005 Almond

(hull) 7

7 1.749

2.827 <0.20

0.366 <0.20

<0.20 <0.20

<0.20 <0.20

<0.20 2.549

3.793

Almond (Nut without shell) 7

7 0.017

<0.010 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 0.057

0.05 RAFNY010 FN205-05H FN205-05H-B USA Dinuba, California 2005 Almond

(hull) 7

7 3.639

3.376 0.779

0.753 0.327

0.303 <0.20

<0.20 <0.20

<0.20 5.145

4.832

Almond (Nut without shell) 7

7 0.011

0.012 0.071

0.051 0.017

0.015 0.025

0.024 0.019

0.010 0.143

0.112 RAFNY010 FN206-05H FN206-05H-A USA Madera, California 2005 Almond

(hull) 7

7 1.759

1.419 <0.20

<0.20 <0.20

<0.20 <0.20

<0.20 <0.20

<0.20 2.559

2.219

Almond (Nut without shell) 7

7 <0.010

<0.010 0.035

0.033 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 0.075

0.073 RAFNY010 FN206-05H FN206-05H-B USA Madera, California 2005 Almond

(hull) 7

7 1.197

0.708 0.225

<0.20 <0.20

<0.20 <0.20

<0.20 <0.20

<0.20 2.022

1.508

Residues (ppm) Study Trial No. Trial SubID Country Year Crop

Portion analysed PHI

(days) BYI

08330 BYI

08330cisenol BYI 08330

ketohydroxy BYI 08330

monohydroxy BYI

08330enolglucoside Total

BYI08330 calc. *

RAFNY010 FN207-05H FN207-05H-A USA Chula, Georgia 2005 Pecan

nut (Nut without shell) 7

7 0.013

0.017 0.012

<0.010 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 0.055

0.057

RAFNY010 FN207-05H FN207-05H-B USA Chula, Georgia 2005 Pecan

nut (Nut without shell) 7

7 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 0.05

0.05

### - 370 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues (ppm) Study Trial No. Trial SubID Country Year Crop

Portion analysed PHI

(days) BYI

08330 BYI

08330cisenol BYI 08330

ketohydroxy BYI 08330

monohydroxy BYI

08330enolglucoside Total

BYI08330 calc. *

RAFNY010 FN208-05H FN208-05H-A USA Nashville, Georgia 2005 Pecan

nut (Nut without shell) 7

7 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 0.05

0.05

RAFNY010 FN208-05H FN208-05H-B USA Nashville, Georgia 2005 Pecan

nut (Nut without shell) 7

7 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 0.05

0.05

RAFNY010 FN209-05H FN209-05H-A USA Proctor, Arkansas 2005 Pecan

nut (Nut without shell) 0

0 7 7 10 10 14 14 21 21 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 0.05

0.05 0.05 0.05 0.05 0.05 0.05 0.05 0.05 0.05

RAFNY010 FN209-05H FN209-05H-B USA Proctor, Arkansas 2005 Pecan

nut (Nut without shell) 7

7 14 14 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.05

0.05 0.05 0.05

RAFNY010 FN210-05H FN210-05H-A USA Wharton, Texas 2005 Pecan

nut (Nut without shell) 7

7 <0.010

<0.010 0.035

0.032 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 0.075

0.072

RAFNY010 FN210-05H FN210-05H-B USA Wharton, Texas 2005 Pecan

nut (Nut without shell) 7

7 <0.010

<0.010 0.122

0.113 <0.010

<0.010 <0.010

0.011 <0.010

<0.010 0.162

0.154

RAFNY010 FN211-05H FN211-05H-A USA D'Hanis, Texas 2005 Pecan

nut (Nut without shell) 7

7 <0.010

<0.010 0.132

0.189 <0.010

0.017 0.015

0.027 <0.010

<0.010 0.177

0.253

### - 371 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues (ppm) Study Trial No. Trial SubID Country Year Crop

Portion analysed PHI

(days) BYI

08330 BYI

08330cisenol BYI 08330

ketohydroxy BYI 08330

monohydroxy BYI

08330enolglucoside Total

BYI08330 calc. *

RAFNY010 FN211-05H FN211-05H-B USA D'Hanis, Texas 2005 Pecan

nut (Nut without shell) 7

7 <0.010

<0.010 0.232

0.237 0.014

0.010 0.031

0.027 <0.010

<0.010 0.297

0.294

### - 372 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

POME FRUIT

Residues (ppm) Study Trial No. Trial SubID Country Year RAC PHI

(days) BYI08330 BYI08330- enol BYI08330-

ketohydroxy BYI08330-

monohydroxy BYI08330-

enolglucoside Total

BYI08330 *

RAFNY009 FN184-05H FN184-05H-A USA North Rose, New York 2005 Apple

fruit 7 7 14 14 0.012

0.016 0.032 0.021 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 0.014 0.010 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.052

0.056 0.076 0.061

RAFNY009 FN184-05H FN184-05H-B USA North Rose, New York 2005 Apple

fruit 7 7 14 14 0.021

0.021 0.022 0.022 0.011

0.012 0.013 0.013 0.016

0.020 0.026 0.022 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.068

0.073 0.081 0.077

RAFNY009 FN185-05H FN185-05H-A USA Hereford, Pennsylvania 2005 Apple

fruit 7 7 14 14 0.084

0.114 0.078 0.095 0.012

0.017 0.016 0.016 0.016

0.020 0.021 0.022 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.132

0.171 0.135 0.153

RAFNY009 FN185-05H FN185-05H-B USA Hereford, Pennsylvania 2005 Apple

fruit 7 7 14 14 0.070

0.064 0.040 0.044 0.018

0.019 0.013 0.013 0.026

0.024 0.022 0.023 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.134

0.127 0.095 0.1

RAFNY009 FN186-05H FN186-05H-A USA Batesville, Virginia 2005 Apple

fruit 7 7 14 14 0.049

0.051 0.034 0.021 0.020

0.021 0.015 <0.010 0.018

0.033 0.011 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.107

0.125 0.08 0.061

RAFNY009 FN186-05H FN186-05H-B USA Batesville, Virginia 2005 Apple

fruit 7 7 14 14 0.034

0.027 0.020 0.027 0.012

<0.010 <0.010 0.012 0.065

0.082 0.056 0.055 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.131

0.139 0.106 0.114

RAFNY009 FN187-05H FN187-05H-A USA Blairsville, Georgia 2005 Apple

fruit 7 7 14 14 0.054

0.056 0.022 0.020 0.017

0.016 <0.010 <0.010 0.017

0.020 0.016 0.014 0.012

0.012 0.011 <0.010 <0.010

<0.010 <0.010 <0.010 0.11

0.114 0.069 0.064

### - 373 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues (ppm) Study Trial No. Trial SubID Country Year RAC PHI

(days) BYI08330 BYI08330- enol BYI08330-

ketohydroxy BYI08330-

monohydroxy BYI08330-

enolglucoside Total

BYI08330 *

RAFNY009 FN187-05H FN187-05H-B USA Blairsville, Georgia 2005 Apple

fruit 7 7 14 14 0.044

0.039 0.018 0.019 0.023

0.022 0.016 0.017 0.029

0.028 0.029 0.025 0.020

0.022 0.021 0.023 <0.010

<0.010 <0.010 <0.010 0.126

0.121 0.094 0.094

RAFNY009 FN188-05HAFN188-05HAA USA Conklin, Michigan 2005 Apple

fruit 7 7 14 14 0.041

0.031 0.031 0.023 <0.010

<0.010 <0.010 <0.010 0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.081

0.071 0.071 0.063

RAFNY009 FN188-05HAFN188-05HAB USA Conklin, Michigan 2005 Apple

fruit 7 7 14 14 0.022

0.025 0.018 0.018 0.011

<0.010 <0.010 0.011 <0.010

<0.010 0.013 0.017 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.063

0.065 0.061 0.066

RAFNY009 FN189-05H FN189-05H-A Canada Simcoe, Ontario 2005 Apple

fruit 7 7 14 14 0.012

0.016 0.016 0.018 0.014

0.014 0.018 0.019 <0.010

<0.010 0.011 0.013 <0.010

<0.010 <0.010 0.011 <0.010

<0.010 <0.010 <0.010 0.056

0.06 0.065 0.071

RAFNY009 FN189-05H FN189-05H-B Canada Simcoe, Ontario 2005 Apple

fruit 7 7 14 14 0.014

0.015 0.011 <0.010 0.022

0.023 0.017 0.019 0.017

0.013 0.012 0.012 0.011

0.012 0.012 0.012 <0.010

<0.010 <0.010 <0.010 0.074

0.073 0.062 0.063

RAFNY009 FN190-05H FN190-05H-A USA, Perry, Utah 2005 Apple

fruit 7 7 14 14 0.081

0.088 0.066 0.061 0.039

0.034 0.042 0.039 0.017

0.012 0.020 0.025 0.022

0.017 0.018 0.021 <0.010

<0.010 <0.010 <0.010 0.169

0.161 0.156 0.156

RAFNY009 FN190-05H FN190-05H-B USA Perry, Utah 2005 Apple

fruit 7 7 14 14 0.108

0.085 0.066 0.059 0.093

0.078 0.096 0.078 0.095

0.068 0.093 0.081 0.069

0.063 0.067 0.062 <0.010

<0.010 <0.010 <0.010 0.375

0.304 0.332 0.29

RAFNY009 FN191-05H FN191-05H-A USA Fresno, California 2005 Apple

fruit 7 7 13 13 0.276

0.316 0.221 0.230 0.010

0.016 <0.010 <0.010 <0.010

0.011 <0.010 <0.010 0.014

0.016 0.019 0.012 <0.010

<0.010 <0.010 <0.010 0.32

0.369 0.27 0.272

### - 374 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues (ppm) Study Trial No. Trial SubID Country Year RAC PHI

(days) BYI08330 BYI08330- enol BYI08330-

ketohydroxy BYI08330-

monohydroxy BYI08330-

enolglucoside Total

BYI08330 *

RAFNY009 FN192-05H FN192-05H-A USA Payette, Idaho 2005 Apple

fruit 0 0 7 7 9 9 14 14 21 21 0.206

0.287 0.218 0.236 0.228 0.417 0.103 0.102 0.104 0.078 0.055

0.055 0.053 0.057 0.073 0.075 0.057 0.055 0.056 0.040 0.017

0.023 0.024 0.030 0.039 0.042 0.032 0.026 0.039 0.027 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 0.298

0.385 0.315 0.343 0.36 0.554 0.212 0.203 0.219 0.165 RAFNY009 FN192-05H FN192-05H-B USA Payette, Idaho 2005 Apple

fruit 7 7 14 14 0.104

0.097 0.052 0.062 0.086

0.086 0.089 0.093 0.044

0.045 0.051 0.055 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.254

0.248 0.212 0.23

RAFNY009 FN193-05H FN193-05H-A USA Parkdale, Oregon 2005 Apple

fruit 7 7 14 14 0.026

0.027 0.015 0.022 0.028

0.028 0.020 0.022 0.019

0.018 0.025 0.024 0.011

<0.010 <0.010 0.010 <0.010

<0.010 <0.010 <0.010 0.094

0.093 0.08 0.088

RAFNY009 FN193-05H FN193-05H-B USA, Parkdale, Oregon; 2005 Apple

fruit 7 7 14 14 0.029

0.030 0.026 0.024 0.073

0.064 0.055 0.054 0.046

0.042 0.041 0.041 0.025

0.024 0.023 0.021 <0.010

<0.010 <0.010 <0.010 0.183

0.17 0.155 0.15

RAFNY009 FN194-05H FN194-05H-A USA Ephrata, Washington 2005 Apple

fruit 7 7 14 14 0.095

0.111 0.095 0.077 0.030

0.031 0.034 0.029 0.016

0.017 0.023 0.020 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.161

0.179 0.172 0.146

RAFNY009 FN194-05H FN194-05H-B USA Ephrata, Washington; 2005 Apple

fruit 7 7 14 14 0.039

0.052 0.026 0.033 0.035

0.037 0.027 0.030 0.022

0.024 0.024 0.022 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.116

0.133 0.097 0.105

RAFNY009 FN195-05H FN195-05H-B USA Hood River, Oregon; 2005 Apple

fruit 7 7 14 14 0.057

0.038 0.031 0.029 0.023

0.014 0.023 0.018 0.015

0.011 0.017 0.015 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.115

0.083 0.091 0.082

### - 375 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues (ppm) Study Trial No. Trial SubID Country Year RAC PHI

(days) BYI08330 BYI08330- enol BYI08330-

ketohydroxy BYI08330-

monohydroxy BYI08330-

enolglucoside Total

BYI08330 *

RAFNY009 FN196-05H FN196-05H-A USA Orefield, Pennsylvania 2005 Pear

fruit 7 7 14 14 0.019

0.022 0.034 0.030 <0.010

<0.010 <0.010 <0.010 0.024

0.028 0.029 0.036 0.017

0.019 0.017 0.017 <0.010

<0.010 <0.010 <0.010 0.08

0.089 0.1 0.103

RAFNY009 FN196-05H FN196-05H-B USA Orefield, Pennsylvania 2005 Pear

fruit 7 7 14 14 0.041

0.037 0.065 0.073 <0.010

<0.010 <0.010 0.011 0.037

0.036 0.040 0.047 0.022

0.022 0.020 0.020 <0.010

<0.010 <0.010 <0.010 0.12

0.115 0.145 0.161

RAFNY009 FN197-05H FN197-05H-A USA Madera, California 2005 Pear

fruit 0 0 7 7 10 10 14 14 21 21 0.177

0.151 0.142 0.088 0.099 0.095 0.060 0.093 0.074 0.101 0.171

0.127 0.148 0.119 0.147 0.167 0.127 0.145 0.097 0.114 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 0.015

0.012 0.018 0.012 0.020 0.022 0.023 0.023 0.027 0.027 0.383

0.31 0.328 0.239 0.286 0.304 0.23 0.281 0.218 0.262 RAFNY009 FN197-05H FN197-05H-B USA Madera, California 2005 Pear

fruit 7 7 14 14 0.098

0.121 0.084 0.079 0.170

0.195 0.148 0.137 0.012

0.016 0.013 0.013 <0.010

<0.010 <0.010 <0.010 0.026

0.031 0.031 0.030 0.316

0.373 0.286 0.269

RAFNY009 FN198-05H FN198-05H-A USA Marysville, California 2005 Pear

fruit 7 7 14 14 0.108

0.164 0.114 0.101 <0.010

<0.010 <0.010 <0.010 0.015

0.020 0.015 0.014 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.153

0.214 0.159 0.145

RAFNY009 FN198-05H FN198-05H-B USA Marysville, California 2005 Pear

fruit 7 7 14 14 0.083

0.098 0.072 0.087 <0.010

<0.010 <0.010 <0.010 0.016

0.017 0.013 0.015 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.129

0.145 0.115 0.132

RAFNY009 FN199-05H FN199-05H-B USA Ephrata, Washington 2005 Pear

fruit 7 7 14 14 0.100

0.114 0.052 0.082 <0.010

<0.010 <0.010 <0.010 0.025

0.025 0.014 0.018 0.058

0.059 0.043 0.050 <0.010

<0.010 <0.010 <0.010 0.203

0.218 0.129 0.17

### - 376 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues (ppm) Study Trial No. Trial SubID Country Year RAC PHI

(days) BYI08330 BYI08330- enol BYI08330-

ketohydroxy BYI08330-

monohydroxy BYI08330-

enolglucoside Total

BYI08330 *

RAFNY009 FN200-05H FN200-05H-A USA Parkdale, Oregon 2005 Pear

fruit 7 7 14 14 0.146

0.143 0.124 0.124 <0.010

<0.010 <0.010 <0.010 0.029

0.024 0.016 0.023 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.205

0.197 0.17 0.177

RAFNY009 FN200-05H FN200-05H-B USA Parkdale, Oregon 2005 Pear

fruit 7 7 14 14 0.117

0.127 0.153 0.087 <0.010

<0.010 <0.010 <0.010 0.064

0.057 0.052 0.050 0.012

0.013 0.016 0.013 <0.010

<0.010 <0.010 <0.010 0.213

0.217 0.241 0.17

RAFNY009 FN201-05H FN201-05H-A USA Hood River, Oregon; 2005 Pear

fruit 7 7 14 14 0.065

0.056 0.065 0.042 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010

0.012 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.105

0.098 0.105 0.082

RAFNY009 FN201-05H FN201-05H-B USA Hood River, Oregon; 2005 Pear

fruit 7 7 14 14 0.022

0.021 0.022 0.014 <0.010

<0.010 <0.010 <0.010 0.010

<0.010 <0.010 <0.010 0.011

0.015 0.011 <0.010 <0.010

<0.010 <0.010 <0.010 0.063

0.066 0.063 0.054

### - 377 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

STONE FRUIT Residues (ppm) Study Trial No. Trial SubID Country Year Crop

Portion analysed DALT a

(days) BYI

08330 BYI

08330cisenol BYI 08330

cis-ketohydroxy BYI

08330

monohydroxy BYI

08330enolglucoside Total

BYI08330 *

RAFNY001 FN146-05H FN146-05H-A USA East Williamson, New York 2005 Peach, fruit Cresthaven 7

7 14 14 0.099

0.239 0.091 0.078 0.163

0.237 0.158 0.145 <0.010

0.012 0.013 <0.010 0.022

0.034 0.048 0.028 <0.020

0.028 0.038 0.027 0.314

0.55 0.348 0.288

RAFNY001 FN146-05H FN146-05H-A USA East Williamson, New York 2005 Peach, fruit Cresthaven 7

7 14 14 0.042

0.047 0.064 0.024 0.554

0.431 0.539 0.394 0.028

0.015 0.017 0.019 0.056

0.053 0.032 0.086 0.020

<0.020 <0.020 0.041 0.7

0.566 0.672 0.564

RAFNY001 FN147-05D FN147-05D-A USA Chula, Georgia 2005 Peach, fruit Hawthorne 7

7 14 14 0.019

0.014 0.018 0.043 0.372

0.473 0.217 0.323 0.013

<0.010 <0.010 0.014 0.086

0.045 0.047 0.059 <0.020

<0.020 0.024 0.037 0.51

0.562 0.316 0.476

RAFNY001 FN147-05D FN147-05D-A USA Chula, Georgia 2005 Peach, fruit Hawthorne 7

7 14 14 0.012

<0.010 <0.010 <0.010 0.320

0.261 0.122 0.212 0.015

<0.010 <0.010 0.011 0.054

0.035 0.032 0.056 0.021

<0.020 0.025 0.030 0.422

0.336 0.199 0.319

RAFNY001 FN148-05H FN148-05H-A USA Plains, Georgia 2005 Peach, fruit Redskin 10 7

7 14 14 <0.010

0.013 <0.010 <0.010 0.187

0.184 0.103 0.106 <0.010

<0.010 <0.010 <0.010 0.048

0.041 0.056 0.045 0.047

0.031 0.036 0.027 0.302

0.279 0.215 0.198

RAFNY001 FN148-05H FN148-05H-B USA Plains, Georgia 2005 Peach, fruit Redskin 10 7

7 14 14 <0.010

0.013 <0.010 <0.010 0.375

0.362 0.230 0.192 <0.010

0.011 <0.010 <0.010 0.065

0.075 0.082 0.080 0.048

0.066 0.044 0.036 0.508

0.527 0.376 0.328

RAFNY001 FN149-05H FN149-05H-A USA Goldsboro, North Carolina 2005 Peach, fruit Norman 7

7 14 14 0.029

0.022 0.011 <0.010 0.385

0.242 0.108 0.137 0.015

0.012 <0.010 <0.010 0.083

0.053 0.052 0.057 0.033

<0.020 <0.020 0.030 0.545

0.349 0.201 0.244

RAFNY001 FN149-05H FN149-05H-B USA Goldsboro, North Carolina 2005 Peach, fruit Norman 7

7 14 14 0.028

0.045 0.014 0.014 0.499

0.507 0.145 0.186 0.022

0.034 0.013 <0.010 0.122

0.155 0.106 0.150 0.049

0.080 0.048 0.060 0.72

0.821 0.326 0.42

### - 378 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues (ppm) Study Trial No. Trial SubID Country Year Crop

Portion analysed DALT a

(days) BYI

08330 BYI

08330cisenol BYI 08330

cis-ketohydroxy BYI

08330

monohydroxy BYI

08330enolglucoside Total

BYI08330 *

RAFNY001 FN150-05D FN150-05D-A USA Beamsville, Ontario 2005 Peach, fruit Canadian Harmony 7

7 14 14 0.010

0.013 <0.010 <0.010 0.327

0.310 0.116 0.268 <0.010

<0.010 <0.010 <0.010 0.016

0.027 <0.010 0.028 0.040

0.053 0.030 0.049 0.403

0.413 0.176 0.365

RAFNY001 FN150-05D FN150-05D-B USA Beamsville, Ontario 2005 Peach, fruit Canadian Harmony 7

7 14 14 <0.010

<0.010 <0.010 <0.010 0.305

0.521 0.277 0.086 0.016

0.025 0.015 <0.010 0.046

0.093 0.040 <0.010 0.037

0.041 0.039 0.049 0.414

0.69 0.381 0.165

RAFNY001 FN151-05H FN151-05H-A USA Waller, Texas 2005 Peach, fruit Texas Royal 7

7 14 14 0.047

0.056 0.026 0.023 0.628

0.942 0.338 0.396 0.017

0.022 0.013 0.015 0.108

0.164 0.152 0.171 0.041

0.043 0.049 0.045 0.841

1.227 0.578 0.65

RAFNY001 FN151-05H FN151-05H-B USA Waller, Texas 2005 Peach, fruit Texas Royal 7

7 14 14 0.056

0.038 0.014 0.019 0.742

0.841 0.487 0.425 0.032

0.025 0.016 0.020 0.160

0.168 0.198 0.214 0.085

0.070 0.055 0.056 1.075

1.142 0.77 0.734

RAFNY001 FN152-05H FN152-05H-B USA Fresno, California 2005 Peach, fruit OHenry 7

7 14 14 0.044

0.077 0.043 0.048 0.362

0.503 0.419 0.324 <0.010

0.010 <0.010 <0.010 0.053

0.077 0.082 0.092 0.021

0.026 0.019 0.025 0.49

0.693 0.573 0.499

RAFNY001 FN153-05H FN153-05H-A USA Selma, California 2005 Peach, fruit Ryan Sun 7

7 14 14 0.161

0.113 0.068 0.164 0.280

0.229 0.088 0.137 <0.010

<0.010 <0.010 <0.010 0.057

0.054 0.034 0.043 0.026

<0.020 <0.020 <0.020 0.534

0.426 0.22 0.374

RAFNY001 FN153-05H FN153-05H-B USA Selma, California 2005 Peach, fruit Ryan Sun 7

7 14 14 0.052

0.069 0.035 0.047 0.366

0.516 0.292 0.229 <0.010

0.010 <0.010 <0.010 0.101

0.131 0.119 0.117 0.028

0.040 <0.020 0.021 0.557

0.766 0.476 0.424

RAFNY001 FN154-05H FN154-05H-A USA Live Oak, California 2005 Peach, fruit Halfords 7

7 14 14 0.108

0.123 0.076 0.071 0.194

0.240 0.098 0.108 <0.010

<0.010 <0.010 <0.010 0.037

0.044 0.031 0.036 <0.020

<0.020 <0.020 <0.020 0.369

0.437 0.235 0.245

RAFNY001 FN154-05H FN154-05H-B USA Live Oak, California 2005 Peach, fruit Halfords 7

7 14 14 0.091

0.093 0.096 0.059 0.350

0.586 0.369 0.273 <0.010

<0.010 0.012 0.011 0.038

0.064 0.073 0.077 <0.020

<0.020 0.021 0.023 0.509

0.773 0.571 0.443

### - 379 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues (ppm) Study Trial No. Trial SubID Country Year Crop

Portion analysed DALT a

(days) BYI

08330 BYI

08330cisenol BYI 08330

cis-ketohydroxy BYI

08330

monohydroxy BYI

08330enolglucoside Total

BYI08330 *

RAFNY001 FN152-05D FN152-05H-B USA Fresno, California 2005 Peach, fruit OHenry 0

0 7 7 7 7 10 10 14 14 14 14 21 21 0.101

0.083 0.044 0.077 0.024 0.034 0.002 0.002 0.043 0.048 0.052 0.051 0.044 0.054 0.222

0.231 0.362 0.503 0.237 0.178 0.003 0.003 0.419 0.324 0.184 0.248 0.170 0.134 0.007

0.005 0.006 0.010 0.005 0.002 0.002 0.002 0.007 0.002 0.002 0.002 0.005 0.002 0.060

0.071 0.053 0.077 0.062 0.051 0.003 0.003 0.082 0.092 0.049 0.105 0.126 0.067 0.018

0.022 0.021 0.026 0.048 0.008 0.008 0.008 0.020 0.025 0.025 0.025 0.017 0.015 0.408

0.412 0.486 0.693 0.376 0.273 0.018 0.018 0.571 0.491 0.312 0.431 0.362 0.272



### PLUM

Residues (ppm) Study Trial No. Trial SubID Country Year Crop

Portion analysed DALT a

(days) BYI

08330 BYI

08330cisenol BYI

08330cis-ketohydroxy BYI

08330

monohydroxy BYI

08330enolglucosid

e Total BYI08330 *

RAFNY001 FN155-05H FN155-05H-A USA Conklin, Michigan 2005 Plum, fruit Stanley 7

7 14 14 <0.01

0 <0.01 0 0.047 0.076 0.116

0.248 0.260 0.169 <0.010

<0.010 <0.010 <0.010 0.048

0.057 0.099 0.069 0.019

0.023 0.041 0.029 0.203

0.348 0.457 0.353

RAFNY001 FN155-05H FN155-05H-B USA Conklin, Michigan 2005 Plum, fruit Stanley 7

7 14 14 <0.01

0 <0.01 0 0.030 0.035 0.582

0.349 0.466 0.382 0.021

0.019 0.019 0.017 0.164

0.103 0.193 0.143 0.065

0.042 0.067 0.058 0.842

0.523 0.775 0.635

RAFNY001 FN156-05D FN156-05D-A USA Selma, California 2005 Plum, fruit September Sun 0

0 7 7 10 10 14 14 21 21 0.017

0.036 0.027 0.038 <0.01 0 0.022 <0.01 0 <0.01 0 0.015 0.014 0.058

0.111 0.290 0.145 0.079 0.294 0.073 0.090 0.047 0.073 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

0.011 0.036 0.015 0.017 0.071 0.021 0.018 0.025 0.040 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 0.105

0.178 0.373 0.218 0.126 0.407 0.124 0.138 0.107 0.147

RAFNY001 FN156-05D FN156-05D-B USA Selma, California 2005 Plum, fruit September Sun 7

7 14 14 <0.01

0 <0.01 0 <0.01 0 <0.01 0 0.211

0.189 0.144 0.092 <0.010

<0.010 <0.010 <0.010 0.037

0.036 0.067 0.036 <0.010

<0.010 <0.010 <0.010 0.278

0.255 0.241 0.158

### - 380 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues (ppm) Study Trial No. Trial SubID Country Year Crop

Portion analysed DALT a

(days) BYI

08330 BYI

08330cisenol BYI

08330cis-ketohydroxy BYI

08330

monohydroxy BYI

08330enolglucosid

e Total BYI08330 *

RAFNY001 FN157-05H FN157-05H-A USA Orlando, California 2005 Plum, fruit French Prune 7

7 14 14 0.029

0.040 0.037 0.044 0.068

0.090 0.098 0.111 <0.010

<0.010 <0.010 <0.010 0.076

0.082 0.127 0.185 <0.010

<0.010 0.012 0.011 0.193

0.232 0.284 0.361

RAFNY001 FN157-05H FN157-05H-B USA Orlando, California 2005 Plum, fruit French Prune 7

7 14 14 0.026

0.029 0.029 0.030 0.046

0.046 0.062 0.076 <0.010

<0.010 <0.010 <0.010 0.062

0.074 0.120 0.113 <0.010

<0.010 <0.010 <0.010 0.154

0.169 0.231 0.239

RAFNY001 FN158-05H FN158-05H-A USA Sanger, California 2005 Plum, fruit Catalina 7

7 14 14 <0.01

0 <0.01 0 <0.01 0 <0.01 0 0.254

0.197 0.253 0.153 <0.010

<0.010 <0.010 <0.010 0.057

0.029 0.118 0.072 0.021

0.013 0.073 0.037 0.352

0.259 0.464 0.282

RAFNY001 FN158-05H FN158-05H-B USA Sanger, California 2005 Plum, fruit Catalina 7

7 14 14 <0.01

0 <0.01 0 <0.01 0 <0.01 0 0.073

0.086 0.057 0.039 <0.010

<0.010 <0.010 <0.010 0.014

0.015 0.019 0.013 <0.010

<0.010 0.010 <0.010 0.117

0.131 0.106 0.082

RAFNY001 FN159-05H FN159-05H-A USA Reedley, California 2005 Plum, fruit 92503 Golden Baby 0

0 7 7 0.010

<0.01 0 <0.01 0 <0.01 0 0.019

0.023 0.013 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.059

0.063 0.053 0.05

RAFNY001 FN159-05H FN159-05H-B USA Reedley, California 2005 Plum, fruit 92503 Golden Baby 7

7 14 14 <0.01

0 <0.01 0 <0.01 0 <0.01 0 0.056

0.048 0.036 0.020 <0.010

<0.010 <0.010 <0.010 0.020

0.013 0.031 <0.010 <0.010

<0.010 <0.010 <0.010 0.106

0.091 0.097 0.06

RAFNY001 FN160-05H FN160-05H-A USA Forest Grove, Oregon 2005 Plum, fruit Mory 7

7 14 14 0.028

0.018 0.023 0.032 0.169

0.081 0.162 0.136 <0.010

<0.010 <0.010 <0.010 0.132

0.067 0.148 0.175 0.015

<0.010 0.015 0.016 0.354

0.186 0.358 0.369

RAFNY001 FN160-05H FN160-05H-B USA Forest Grove, Oregon 2005 Plum, fruit Mory 7

7 14 14 0.021

0.024 0.021 <0.01 0 0.315

0.277 0.311 0.120 <0.010

<0.010 0.011 <0.010 0.200

0.190 0.343 0.146 0.024

0.024 0.041 0.021 0.57

0.525 0.727 0.307

### - 381 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

CHERRY Residues (ppm) Study Trial No. Trial SubID GLP Year Crop

Variety PHI

(days) BYI

08330 BYI 08330

cis-enol BYI

08330cis-ketohydroxy BYI

08330

monohydroxy BYI

08330enolglucoside Total

BYI08330 calc. *

RAFNY001 FN140-05H FN140-05H-A GLP yes 2005 Cherry,

sour Mont Morency 7

7 14 14 0.056

0.075 <0.010 <0.010 1.026

0.876 0.682 0.455 0.036

0.045 0.049 0.085 0.219

0.301 0.275 0.487 0.271

0.204 0.345 0.401 1.608

1.501 1.361 1.438

RAFNY001 FN140-05H FN140-05H-B GLP yes 2005 Cherry,

sour Mont Morency 7

7 14 14 0.017

<0.010 <0.010 <0.010 1.32

1.08 0.780 0.678 0.086

0.051 0.055 0.074 0.402

0.227 0.340 0.370 0.302

0.253 0.337 0.359 2.127

1.621 1.522 1.491

RAFNY001 FN141-05H FN141-05H-A GLP yes 2005 Cherry,

sour Mont Morency 7

7 14 14 0.043

0.060 0.031 0.015 1.28

1.29 0.861 0.03 0.044

0.055 0.045 0.053 0.102

0.115 0.154 0.174 0.092

0.106 0.120 0.115 1.561

1.626 1.211 0.387

RAFNY001 FN141-05H FN141-05H-B GLP yes 2005 Cherry,

sour Mont Morency 7

7 14 14 0.015

0.011 <0.010 0.010 1.13

1.08 0.573 0.659 0.053

0.060 0.053 0.091 0.117

0.127 0.194 0.272 0.100

0.085 0.137 0.211 1.415

1.363 0.967 1.243

RAFNY001 FN142-05H FN142-05H-A GLP yes 2005 Cherry,

sour Mont Morency 7

7 14 14 0.016

0.022 0.011 0.027 1.38

1.61 1.38 1.50 0.062

0.065 0.065 0.073 0.223

0.218 0.201 0.265 0.231

0.205 0.275 0.321 1.912

2.12 1.932 2.186

RAFNY001 FN142-05H FN142-05H-B GLP yes 2005 Cherry,

sour Mont Morency 7

7 14 14 0.012

0.012 <0.010 <0.010 1.22

1.23 0.676 0.738 0.100

0.096 0.055 0.059 0.332

0.356 0.236 0.231 0.368

0.362 0.266 0.236 2.032

2.056 1.243 1.274

RAFNY001 FN143-05H FN143-05H-A GLP yes 2005 Cherry,

sweet Bing 7

7 14 14 0.078

0.089 0.07 0.067 0.434

0.592 0.508 0.592 0.031

0.037 0.04 0.04 0.011

0.022 0.029 0.024 <0.010

<0.010 <0.010 <0.010 0.564

0.75 0.657 0.733

RAFNY001 FN143-05H FN143-05H-B GLP yes 2005 Cherry,

sweet Bing 7

7 14 14 0.035

0.012 0.016 0.058 0.529

0.17 0.247 0.383 0.02

0.02 0.015 0.034 <0.010

<0.010 0.023 0.023 <0.010

<0.010 <0.010 <0.010 0.604

0.222 0.311 0.508

RAFNY001 FN144-05H FN144-05H-A GLP yes 2005 Cherry,

sweet Bing 7

7 14 14 0.062

0.035 0.056 0.068 0.868

0.846 0.838 0.818 0.051

0.035 0.051 0.045 0.110

0.090 0.179 0.189 0.038

0.030 0.051 0.056 1.129

1.036 1.175 1.176

RAFNY001 FN144-05H FN144-05H-B GLP yes 2005 Cherry,

sweet Bing 7

7 14 14 0.014

0.015 0.013 0.014 1.22

1.29 0.96 1.08 0.052

0.069 0.052 0.091 0.147

0.197 0.185 0.246 0.044

0.063 0.077 0.098 1.477

1.634 1.287 1.529

### - 382 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues (ppm) Study Trial No. Trial SubID GLP Year Crop

Variety PHI

(days) BYI

08330 BYI 08330

cis-enol BYI

08330cis-ketohydroxy BYI

08330

monohydroxy BYI

08330enolglucoside Total

BYI08330 calc. *

RAFNY001 FN145-05H FN145-05H-A GLP yes 2005 Cherry,

sweet Bing 0

0 7 7 10 10 14 14 21 21 0.992

0.997 0.026 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 0.803

0.811 0.832 0.251 0.095 0.052 0.055 0.092 0.05 0.04 0.043

0.044 0.059 0.011 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 0.073

0.077 0.127 0.036 0.03 <0.010 0.014 0.02 <0.010 <0.010 0.016

0.012 0.018 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 1.927

1.941 1.062 0.318 0.155 0.092 0.099 0.142 0.09 0.08 RAFNY001 FN145-05H FN145-05H-B GLP yes 2005 Cherry,

sweet Bing 7

7 14 14 0.018

0.018 0.010 <0.010 1.23

1.28 0.775 0.678 0.087

0.065 0.069 0.053 0.200

0.223 0.262 0.222 0.047

0.044 0.055 0.040 1.582

1.63 1.171 1.003

RAFNY001 FN144-05H FN144-05H-C GLP yes 2005 Cherry,

sweet Bing 7

7 14 14 0.073

0.061 0.051 0.073 0.487

0.433 0.387 0.576 0.022

0.019 0.014 0.024 0.046

0.044 0.042 0.081 0.018

0.015 0.015 0.026 0.646

0.572 0.509 0.78

### - 383 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

GRAPES

Residues (ppm) Study Trial No. Trial SubID Country Year RAC PHI (days) BYI

08330 BYI

08330cisenol BYI

08330- ketohydroxy BYI

08330

monohydroxy BYI 08330

enolglucoside Total

BYI08330 *

RAFNY011 FN212-05H USA Orefield, Pennsylvania 2005 Table grape

berry, table grape 7

7 14 14 0.094

0.091 0.013 <0.010 0.106

0.120 0.029 0.019 0.013

0.011 <0.010 <0.010 0.011

<0.010 <0.010 <0.010 0.095

0.089 0.030 0.023 0.319

0.321 0.092 0.072

RAFNY011 FN213-05H FN213-05H-A USA, Dundee, New York, 2005 Table grape

berry, table grape 7

7 14 14 0.126

0.174 0.080 0.133 0.378

0.404 0.234 0.331 0.012

0.019 <0.010 0.013 0.036

0.046 0.038 0.042 0.111

0.144 0.109 0.162 0.663

0.787 0.471 0.681

RAFNY011 FN214-05D USA Fresno, California 2005 Table grape

berry, table grape 3

3 7 7 10 10 14 14 21 21 0.055

0.074 0.066 0.076 0.073 0.046 0.102 0.103 0.062 0.062 0.072

0.078 0.093 0.107 0.095 0.088 0.163 0.161 0.100 0.116 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 0.028

0.032 0.037 0.038 0.025 0.021 0.057 0.064 0.058 0.055 0.175

0.204 0.216 0.241 0.213 0.175 0.342 0.348 0.24 0.253 RAFNY011 FN215-05H FN215-05H-A USA Plainview, California, 2005 Table grape

berry, table grape 7

7 14 14 0.133

0.189 0.136 0.134 0.044

0.048 0.054 0.063 0.020

0.016 0.014 0.016 <0.010

<0.010 <0.010 <0.010 0.020

0.029 0.025 0.025 0.227

0.292 0.239 0.248

RAFNY011 FN216-05H USA Sanger, California 2005 Table grape

berry, table grape 7

7 14 14 0.062

0.058 0.029 0.037 0.077

0.076 0.043 0.055 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.080

0.108 0.058 0.107 0.239

0.262 0.15 0.219

RAFNY011 FN217-05H USA Artois, California 2005 Table grape

berry, table grape 7

7 13 13 0.035

0.041 0.034 0.042 0.018

0.016 0.019 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.038

0.032 0.060 0.038 0.111

0.109 0.133 0.11

RAFNY011 FN218-05H USA Orcutt, California 2005 Grapes

(Wine) Chardonnay 7

7 14 14 0.046

0.061 0.064 0.074 0.148

0.258 0.223 0.225 0.013

0.019 0.022 0.018 <0.010

<0.010 <0.010 <0.010 0.092

0.127 0.170 0.148 0.309

0.475 0.489 0.475

RAFNY011 FN219-05H USA Hughson, California 2005 Table grape

berry, table grape 7

7 14 14 0.156

0.203 0.194 0.181 0.174

0.175 0.295 0.197 0.011

0.013 0.028 0.020 <0.010

<0.010 <0.010 <0.010 0.089

0.099 0.127 0.102 0.44

0.5 0.654 0.51

### - 384 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues (ppm) Study Trial No. Trial SubID Country Year RAC PHI (days) BYI

08330 BYI

08330cisenol BYI

08330- ketohydroxy BYI

08330

monohydroxy BYI 08330

enolglucoside Total

BYI08330 *

RAFNY011 FN220-05H FN220-05H-A USA Fresno, California 2005 Table grape

berry, table grape 7

7 14 14 0.114

0.199 0.203 0.087 0.079

0.082 0.113 0.063 <0.010

<0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.036

0.035 0.059 0.036 0.249

0.336 0.395 0.206

RAFNY011 FN221-05H USA Paso Robles, California 2005 Table grape

berry, table grape 7

7 14 14 0.149

0.180 0.332 0.369 0.116

0.151 0.243 0.256 0.023

0.024 0.040 0.045 <0.010

<0.010 <0.010 <0.010 0.083

0.106 0.144 0.163 0.381

0.471 0.769 0.843

RAFNY011 FN222-05H USA Ephrata, Washington 2005 Table grape

berry, table grape 7

7 14 14 0.494

0.209 0.246 0.216 0.503

0.344 0.347 0.369 0.206

0.120 0.115 0.090 <0.010

<0.010 <0.010 <0.010 0.077

0.074 0.074 0.088 1.29

0.757 0.792 0.773

RAFNY011 FN223-05H USA Hood River, Oregon 2005 Table grape

berry, table grape 7

7 14 14 0.142

0.128 0.130 0.151 0.158

0.167 0.232 0.155 0.015

0.011 0.022 0.018 <0.010

<0.010 0.012 <0.010 0.053

0.048 0.084 0.064 0.378

0.364 0.48 0.398

### - 385 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

TOMATO

Residues (ppm) Study Trial No. Trial SubID Location Year RAC PHI (days) BYI08330 BYI08330- enol BYI08330-

ketohydroxy BYI08330-

monohydroxy BYI08330-

enolglucoside Total

BYI08330 calc. *

RAFNY006 Tomato 1 <0.010 0.077 <0.010 <0.010 0.016 0 .123 FN045-04H fruit 1 <0.010 0.078 <0.010 <0.010 0.012 0.12 USA 3 <0.010 0.133 <0.010 <0.010 0.031 0.194 Germansville, 3 <0.010 0.101 <0.010 <0.010 0.023 0.154 Pennsylvania 7 <0.010 0.072 <0.010 <0.010 0.021 0.1 23

2004 7 <0.010 0.062 <0.010 <0.010 0.015 0.107 RAFNY006 Tomato 1 0.025 0.052 <0.010 <0.010 <0.010 0 .107 FN046-04H fruit 1 0.021 0.042 <0.010 <0.010 <0.010 0.093

FN046-04H-A 3 <0.010 0.058 <0.010 <0.010 <0.010 0.0 98 USA 3 <0.010 0.047 <0.010 <0.010 <0.010 0.087 Tifton, Georgia 7 <0.010 0.056 <0.010 <0.010 0.021 0.107

2004 7 <0.010 0.068 <0.010 <0.010 0.023 0.121 RAFNY006 Tomato 1 <0.010 0.132 0.01 <0.010 <0.010 0. 172 FN047-04HA fruit 1 <0.010 0.165 0.022 <0.010 <0.010 0.217 USA 3 <0.010 0.13 0.013 <0.010 <0.010 0.173 Molino, 3 <0.010 0.195 <0.010 <0.010 <0.010 0.235

Florida 7 <0.010 0.227 <0.010 <0.010 0.011 0.268

2004 7 <0.010 0.215 0.011 <0.010 0.013 0.259 RAFNY006 Tomato 1 <0.010 0.037 <0.010 <0.010 <0.010 0.077 FN048-04H fruit 1 <0.010 0.032 <0.010 <0.010 <0.010 0.072 USA 3 <0.010 0.034 <0.010 <0.010 <0.010 0.074 Jennings, 3 <0.010 0.032 <0.010 <0.010 <0.010 0.0 72 Florida 7 <0.010 0.086 <0.010 <0.010 0.025 0.141

2004 7 <0.010 0.056 <0.010 <0.010 0.018 0.104 RAFNY006 Tomato 0 0.022 0.027 <0.010 <0.010 <0.010 0 .079 FN049-04DA fruit 0 0.039 0.031 <0.010 <0.010 <0.010 0.1 USA 1 <0.010 0.03 <0.010 <0.010 <0.010 0.07 Stilwell, 1 <0.010 0.02 <0.010 <0.010 <0.010 0.06

Kansas 4 <0.010 0.025 <0.010 <0.010 <0.010 0.065

2004 4 <0.010 0.019 <0.010 <0.010 <0.010 0.059

7 <0.010 0.025 <0.010 <0.010 0.013 0.068

7 <0.010 0.017 <0.010 <0.010 <0.010 0.057

10 <0.010 0.017 <0.010 <0.010 <0.010 0.057

10 <0.010 0.012 <0.010 <0.010 <0.010 0.052 RAFNY006 Tomato 1 0.045 0.086 <0.010 <0.010 <0.010 0 .161 FN050-04H fruit 1 0.034 0.163 <0.010 <0.010 <0.010 0.227 FN050-04H-A 3 0.048 0.104 <0.010 <0.010 <0.010 0.18 2 USA 3 0.043 0.129 <0.010 <0.010 0.011 0.203 Fresno, California 7 0.043 0.153 <0.010 <0.010 0.017 0.233

2004 7 0.035 0.153 <0.010 <0.010 0.018 0.226 RAFNY006 Tomato 1 0.077 0.108 <0.010 <0.010 0.013 0. 218 FN051-04H fruit 1 0.077 0.102 <0.010 <0.010 0.011 0 .21 FN051-04H-A 3 0.062 0.079 <0.010 <0.010 0.013 0.174 USA 3 0.064 0.101 <0.010 <0.010 0.019 0.204 Glenn, California 7 0.06 0.161 <0.010 <0.010 <0.010 0.251

### - 386 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues (ppm) Study Trial No. Trial SubID Location Year RAC PHI (days) BYI08330 BYI08330- enol BYI08330-

ketohydroxy BYI08330-

monohydroxy BYI08330-

enolglucoside Total

BYI08330 calc. *

2004 7 0.072 0.146 <0.010 <0.010 <0.010 0.248 RAFNY006 Tomato 1 0.014 0.1 <0.010 <0.010 <0.010 0.1 44 FN052-04H fruit 1 <0.010 0.103 <0.010 <0.010 <0.010 0.143 USA 4 <0.010 0.11 <0.010 <0.010 <0.010 0.15 Paso Robles, 4 <0.010 0.103 <0.010 <0.010 <0.010 0.143 California 7 <0.010 0.194 <0.010 <0.010 <0.010 0.2 34

2004 7 <0.010 0.202 <0.010 <0.010 <0.010 0.242 RAFNY006 Tomato 1 0.051 0.08 <0.010 <0.010 <0.010 0. 161 FN053-04H fruit 1 0.047 0.092 <0.010 <0.010 <0.010 0.169 USA 3 0.018 0.061 <0.010 <0.010 <0.010 0.109 Visalia, 3 0.012 0.038 <0.010 <0.010 <0.010 0.08 California 7 <0.010 0.046 <0.010 <0.010 <0.010 0.0 86

2004 7 <0.010 0.051 <0.010 <0.010 <0.010 0.091 RAFNY006 Tomato 1 0.012 0.071 <0.010 <0.010 <0.010 0 .113 FN054-04H fruit 1 0.01 0.071 <0.010 <0.010 <0.010 0 .111 USA 3 0.017 0.131 <0.010 <0.010 0.015 0.183 Porterville, 3 0.017 0.133 <0.010 <0.010 0.018 0.1 88 California 7 <0.010 0.129 <0.010 <0.010 0.014 0.17 3

2004 7 <0.010 0.158 <0.010 <0.010 0.021 0.209 RAFNY006 Tomato 1 0.014 0.087 <0.010 <0.010 <0.010 0 .131 FN055-04H fruit 1 0.025 0.123 <0.010 <0.010 0.012 0 .18 USA 3 <0.010 0.098 <0.010 <0.010 <0.010 0.138 Fresno, 3 <0.010 0.086 <0.010 <0.010 <0.010 0.126 California 7 0.016 0.146 <0.010 <0.010 0.016 0.198

2004 7 0.022 0.229 <0.010 <0.010 0.035 0.306 RAFNY006 Tomato 1 0.014 0.063 <0.010 <0.010 <0.010 0 .107 FN056-04H fruit 1 0.025 0.088 <0.010 <0.010 <0.010 0.143 USA 3 0.017 0.058 <0.010 <0.010 <0.010 0.105 Madera, 3 0.013 0.077 <0.010 <0.010 <0.010 0.12 California 7 0.019 0.088 <0.010 <0.010 0.018 0.145

2004 7 0.029 0.087 0.01 <0.010 0.016 0.152



### PEPPER

Residues (ppm) Study Trial No. Trial SubID Country Year RAC PHI

(days) BYI08330 BYI08330- enol BYI08330-

ketohydroxy BYI08330-

monohydroxy BYI08330-

enolglucoside Total

BYI08330 calc. *

RAFNY006 FN057-04D USA Tifton, Georgia 2004 Pepper,

sweet fruit 0

0 1 1 3 3 7 7 10 10 0.011

0.011 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 0.051

0.059 0.093 0.089 0.077 0.099 0.190 0.108 0.087 0.191 0.019

0.023 0.049 0.037 0.045 0.038 0.060 0.053 0.045 0.051 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.022 0.018 0.023 0.033 0.101

0.113 0.172 0.156 0.152 0.167 0.292 0.199 0.175 0.295

### - 387 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues (ppm) Study Trial No. Trial SubID Country Year RAC PHI

(days) BYI08330 BYI08330- enol BYI08330-

ketohydroxy BYI08330-

monohydroxy BYI08330-

enolglucoside Total

BYI08330 calc. *

RAFNY006 FN058-04H FN058- 04H-A USA Molino, Florida 2004 Pepper,

sweet fruit 1

1 3 3 7 7 <0.010

<0.010 0.013 0.014 <0.010 <0.010 0.102

0.148 0.286 0.492 0.361 0.258 0.058

0.092 0.120 0.205 0.145 0.137 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.011

0.017 0.034 0.054 0.057 0.062 0.191

0.277 0.463 0.775 0.583 0.477

RAFNY006 FN059-04H USA Springfield, Nebraska 2004 Pepper,

sweet fruit 1

1 4 4 7 7 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.394

0.232 0.276 0.269 0.242 0.615 0.139

0.112 0.119 0.134 0.083 0.233 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.017

0.016 0.015 0.018 0.020 0.051 0.57

0.38 0.43 0.441 0.365 0.919

RAFNY006 FN060-04H USA East Bernard, Texas 2004 Pepper,

sweet fruit 1

1 3 3 7 7 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.204

0.263 0.204 0.210 0.203 0.247 0.039

0.069 0.037 0.051 0.065 0.036 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.273

0.362 0.271 0.291 0.298 0.313

RAFNY006 FN061-04H FN061- 04H-A USA Fresno, California 2004 Pepper,

sweet fruit 1

1 3 3 7 7 0.025

0.033 0.026 0.016 <0.010 0.014 0.530

0.489 0.690 0.609 0.446 0.749 0.096

0.075 0.078 0.116 0.131 0.229 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.021

0.022 0.031 0.027 0.033 0.068 0.682

0.629 0.835 0.778 0.63 1.07

RAFNY006 FN062-04H USA Hickman, California 2004 Pepper,

sweet fruit 1

1 3 3 7 7 0.046

0.034 0.028 0.049 0.035 0.032 0.208

0.106 0.183 0.374 0.271 0.413 0.047

0.042 0.057 0.050 0.057 0.070 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 0.012 0.013 0.024 0.321

0.202 0.288 0.495 0.386 0.549



### CUCUMBER Residues (mg/kg) Study Trial No. Trial SubID Country GLP Year Crop

Portion analyse d DALT

a (days ) BYI 08330 BYI 08330

cis-enol BYI 08330

cis-ketohydroxy BYI 08330

monohydroxy BYI 08330

enolglucoside Total

Residue of BYI 08330 calc.

RAFNY007 FN066-04H FN066-04H-A Tifton, Georgia 2004 Cucumb

er fruit 1

1 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 <0.050

<0.050

RAFNY007 FN067-04H Louisa, Virginia 2004 Cucumb

er fruit 1

1 <0.010

<0.010 <0.010

<0.010 <0.010

0.033 <0.010

<0.010 <0.010

<0.010 <0.050

0.073

RAFNY007 FN068-04HA Molino, Florida 2004 Cucumb

er fruit 1

1 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 <0.050

<0.050

### - 388 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Residues (mg/kg) Study Trial No. Trial SubID Country GLP Year Crop

Portion analyse d DALT

a (days ) BYI 08330 BYI 08330

cis-enol BYI 08330

cis-ketohydroxy BYI 08330

monohydroxy BYI 08330

enolglucoside Total

Residue of BYI 08330 calc.

RAFNY007 FN069-04D Stilwell, Kansas 2004 Cucumb

er fruit 0

0 1 1 1 6 6 9 9 0.012

0.017 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 0.052

0.057 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050

whole

fruit, washed 1 <0.010 <0.010 <0.010 <0.010 <0.010 <0.050

fruit

without peel 1 <0.010 <0.010 <0.010 <0.010 <0.010 <0.050

RAFNY007 FN070-04H FN070-04H-A Seymour, Illinois 2004 Cucumb

er fruit 1

1 <0.010

<0.010 <0.010

<0.010 0.014

0.017 <0.010

<0.010 <0.010

<0.010 0.054

0.057

RAFNY007 FN071-04H Eagle Lake, Texas 2004 Cucumb

er fruit 1

1 0.034

0.029 <0.010

0.010 0.012

0.014 <0.010

<0.010 <0.010

<0.010 0.076

0.073

Cucumbers- 240 SC formulation

RAFNY007 FN066-04H FN066-04H-B Tifton, Georgia 2004 Cucumb

er fruit 1

1 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 <0.050

<0.050

RAFNY007 FN070-04H FN070-04H-B Seymour, Illinois 2004 Cucumb

er fruit 1

1 <0.010

<0.010 <0.010

<0.010 0.017

<0.010 <0.010

<0.010 <0.010

<0.010 0.057

<0.050



### MELON

RAFNY007 FN072-04HA Molino, Florida 2004 Melon,

cantalo up fruit 1

1 <0.010

<0.010 0.013

<0.010 0.014

<0.010 <0.010

<0.010 <0.010

<0.010 0.057

<0.050

### - 389 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

RAFNY007 FN073-04D Valley, Nebraska 2004 Melon,

cantalo up fruit 0

0 1 1 1 3 3 7 7 10 10 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.050

<0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050

fruit

without peel 1 <0.010 <0.010 <0.010 <0.010 <0.010 <0.050

RAFNY007 FN074-04H Uvalde, Texas 2004 Melon,

cantalo up fruit 2

2 0.069

0.020 0.035

0.012 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 0.134

0.062

RAFNY007 FN075-04H FN075-04H-A Fresno, California 2004 Melon,

cantalo up fruit 1

1 0.028

0.016 0.025

0.018 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 0.083

0.064

RAFNY007 FN076-04H FN076-04H-A El Centro, California 2004 Melon,

cantalo up fruit 1

1 <0.010

0.011 0.016

<0.010 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 0.056

0.051

RAFNY007 FN077-04H Orland, California 2004 Melon,

cantalo up fruit 1

1 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 <0.050

<0.050

Muskmelon – 240 SC formulation

RAFNY007 FN075-04H FN075-04H-B Fresno, California 2004 Melon,

cantalo up fruit 1

1 0.015

<0.010 0.012

<0.010 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 0.057

<0.050

RAFNY007 FN076-04H FN076-04H-B El Centro, California 2004 Melon,

cantalo up fruit 1

1 0.017

0.077 0.016

0.056 <0.010

<0.010 <0.010

<0.010 <0.010

<0.010 0.063

0.163

Summer Squash – 100 OD formulation

RAFNY007 FN078-04H Germansville, Pennsylvania 2004 Squash,

summer fruit 1

1 3 3 7 7 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.078

0.055 0.025 0.016 <0.010 <0.010 0.076

0.076 0.052 0.055 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.184

0.161 0.107 0.101 <0.050 <0.050

### - 390 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

RAFNY007 FN079-04D Tifton, Georgia 2004 Squash,

summer fruit 0

0 1 1 1 3 3 7 7 10 10 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 0.015

<0.010 <0.010 0.011 <0.010 0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 0.055

<0.050 <0.050 0.051 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050 <0.050

fruit,

cooked 1 <0.010 0.021 <0.010 <0.010 <0.010 0.061

fruit

without peel 1 <0.010 <0.010 <0.010 <0.010 <0.010 <0.050

whole

fruit, washed 1 <0.010 <0.010 <0.010 <0.010 <0.010 <0.050

RAFNY007 FN080-04HA Molino, Florida 2004 Squash,

summer fruit 1

1 3 3 7 7 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.014

0.010 <0.010 0.011 <0.010 <0.010 0.033

0.019 0.017 0.033 0.015 0.011 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.077

0.059 0.057 0.074 0.055 0.051

RAFNY007 FN081-04H FN081-04H-A Valley, Nebraska 2004 Squash,

summer fruit 1

1 3 3 7 7 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.013

0.020 0.013 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.053

0.060 0.053 <0.050 <0.050 <0.050

RAFNY007 FN082-04H Fresno, California 2004 Squash,

summer fruit 1

1 3 3 7 7 0.062

0.045 0.077 0.042 <0.010 0.020 0.043

0.034 0.050 0.028 <0.010 0.015 0.017

<0.010 0.014 0.013 <0.010 0.012 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.142

0.109 0.161 0.103 <0.050 0.067

### - 391 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

FLOWERING BRASSICA

Trial ID (City, State/Year) Commodity

or Matrix Total

Rate (lb a.i./A) (kg a.i./ha) PHI

(days) BYI

08330 (ppm) BYI

08330- enol (ppm) BYI 08330-

ketohydroxy (ppm) BYI

08330-

monohydroxy (ppm) BYI

08330-enolGlc (ppm) Total

Residues of BYI 08330 (ppm)

Uvalde, Texas Region 6 Broccoli

flower head 100OD

0.158 (0.177) 1

1 3 3 7 7 0.025

0.030 0.031 0.036 <0.010 <0.010 0.164

0.118 0.278 0.272 0.265 0.229 0.160

0.164 0.382 0.432 0.523 0.459 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 0.040 0.032 0.063 0.071 0.369

0.332 0.741 0.782 0.871 0.779 Uvalde, Texas Region 6 Broccoli

flower head 240

SC 0.157 (0.176) 1

1 3 3 7 7 0.034

0.023 0.024 0.015 0.011 <0.010 0.121

0.118 0.166 0.137 0.229 0.384 0.150

0.127 0.271 0.164 0.377 0.398 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 0.019 0.005 0.045 0.033 0.325

0.288 0.49 0.331 0.672 0.835 Broccoli flower head 0 0 1 1 1 3 3 7 7 10 10 0.123

0.147 0.057 0.056 0.029 0.045 0.065 0.039 0.040 <0.010 <0.010 0.138

0.108 0.128 0.095 0.061 0.089 0.104 0.131 0.171 0.124 0.147 0.272

0.194 0.201 0.216 0.230 0.241 0.209 0.356 0.315 0.328 0.286 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 0.011 0.012 0.015 0.012 0.553

0.469 0.406 0.387 *0.34 0.395 0.398 0.547 0.548 0.487 0.465 head, cooked 1 <0.010 0.314 0.016 <0.010 <0.010 0.360 Fresno, California Region 10

head,

washed 100OD

0.157 (0.176)

1 <0.010 0.055 0.211 <0.010 <0.010 0.296

Hickman, California Region 10 Broccoli

flower head 100OD

0.154 (0.173) 1

1 3 3 7 7 0.022

0.027 <0.010 <0.010 <0.010 <0.010 0.023

0.033 0.051 0.056 0.085 0.068 0.034

0.027 0.053 0.050 0.063 0.068 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.099

0.107 0.134 0.136 0.178 0.166

King City, California Region 10 Cauliflower

flower head 100

OD 0.158 (0.178) 1

1 3 3 7 7 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.093

0.102 0.048 0.059 0.094 0.059 0.201

0.213 0.153 0.131 0.190 0.106 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.324

0.345 0.231 0.22 0.314 0.195

King City, California Region 10 Cauliflower

flower head 240

SC 0.156 (0.176) 1

1 3 3 7 7 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.045

0.065 0.055 0.066 0.028 0.027 0.135

0.194 0.140 0.130 0.098 0.087 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.21

0.289 0.225 0.226 0.156 0.144

### - 392 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Trial ID (City, State/Year) Commodity

or Matrix Total

Rate (lb a.i./A) (kg a.i./ha) PHI

(days) BYI

08330 (ppm) BYI

08330- enol (ppm) BYI 08330-

ketohydroxy (ppm) BYI

08330-

monohydroxy (ppm) BYI

08330-enolGlc (ppm) Total

Residues of BYI 08330 (ppm)

Glenn, California Region 10 Cauliflower

flower head 100

OD 0.155 (0.173) 1

1 3 3 7 7 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.214

0.176 0.227 0.227 0.270 0.230 0.207

0.189 0.178 0.213 0.242 0.245 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.451

0.395 0.435 0.47 0.542 0.505

Corvallis, Oregon Region 12 Cauliflower

flower head 100

OD 0.157 (0.177) 1

1 3 3 7 7 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.063

0.058 0.045 0.056 0.091 0.070 0.318

0.318 0.267 0.219 0.315 0.302 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.010

0.011 0.012 <0.010 0.020 0.019 0.411

0.407 0.344 0.305 0.446 0.411



### HEAD CABBAGE

Trial ID (City, State/Year) Commodity

or Matrix Total

Rate (lb a.i./A) (kg a.i./ha) PHI

(days) BYI

08330 (ppm) BYI

08330- enol (ppm) BYI 08330-

ketohydroxy (ppm) BYI

08330-

monohydroxy (ppm) BYI

08330-enolGlc (ppm) Total

Residues of BYI 08330 (ppm)

Cabbage, field head 1 1 3 3 7 7 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 0.013 0.011 <0.010 <0.010 0.017

0.014 0.024 0.022 0.023 0.020 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 0.011 0.057

0.054 0.067 0.063 0.063 0.061 Tifton, Georgia Region 2

head,

trimmed 100

OD 0.157 (0.176)

1

1 3 3 7 7 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 0.012 <0.010 <0.010 0.022

0.026 0.024 0.015 0.016 0.022 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.062

0.066 0.064 0.057 0.056 0.062 Cabbage, field head 1 1 3 3 7 7 0.757

0.693 0.156 0.084 0.048 0.068 0.129

0.099 0.037 0.026 0.025 0.028 <0.010

0.085 0.079 0.064 0.057 0.054 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.018

<0.010 0.037 0.026 0.025 0.028 0.924

0.897 0.319 0.21 0.165 0.188 Bumpass, VA Region 1

head,

trimmed 100

OD 0.157 (0.176)

1

1 3 3 7 7 0.052

0.034 <0.010 <0.010 <0.010 <0.010 0.035

0.036 0.025 0.030 0.018 0.024 0.063

0.068 0.074 0.075 0.060 0.066 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.17

0.158 0.129 0.135 0.108 0.12 Tifton, Georgia Region 2 Cabbage,

field head 240

SC 0.157 (0.176) 1

1 3 3 7 7 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 0.016 0.011 0.010 0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.05

0.05 0.056 0.051 0.05 0.05

### - 393 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Trial ID (City, State/Year) Commodity

or Matrix Total

Rate (lb a.i./A) (kg a.i./ha) PHI

(days) BYI

08330 (ppm) BYI

08330- enol (ppm) BYI 08330-

ketohydroxy (ppm) BYI

08330-

monohydroxy (ppm) BYI

08330-enolGlc (ppm) Total

Residues of BYI 08330 (ppm)

head, trimmed 1 1 3 3 7 7 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.016

0.015 0.012 0.017 0.020 0.014 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.056

0.055 0.052 0.057 0.06 0.054 Cabbage, field head 1 1 3 3 7 7 0.329

0.303 0.053 0.045 0.059 0.023 0.170

0.157 0.125 0.102 0.151 0.159 0.123

0.166 0.174 0.128 0.217 0.197 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 0.012 0.016 0.642

0.646 0.372 0.295 0.449 0.405 Molino, Florida Region 3

head,

trimmed 100

OD 0.153 (0.171)

1

1 3 3 7 7 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.020

0.029 0.052 0.036 0.055 0.039 0.050

0.052 0.089 0.066 0.088 0.074 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.1

0.111 0.171 0.132 0.173 0.143 Cabbage, field head 0 0 1 1 3 3 7 7 10 10 0.073

0.092 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 0.081

0.096 0.085 0.057 0.061 0.061 0.067 0.044 0.032 0.039 0.107

0.096 0.109 0.097 0.146 0.111 0.131 0.108 0.073 0.101 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 0.018

0.013 0.017 0.015 0.014 0.011 0.021 0.018 0.016 0.026 0.289

0.307 0.231 0.189 0.241 0.203 0.239 0.19 0.141 0.186 head, cooked 1 <0.010 0.124 <0.010 <0.010 <0.010 0.164 Stilwell, Kansas Region 5

head,

trimmed 100

OD 0.158 (0.178)

1 <0.010 0.026 0.059 <0.010 0.011 0.116

Cabbage, field head 1 1 3 3 7 7 0.182

0.123 0.113 0.140 <0.010 0.011 0.090

0.088 0.102 0.093 0.040 0.040 0.156

0.162 0.209 0.256 0.096 0.127 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 0.011 0.016 0.014 0.016 0.448

0.393 0.445 0.515 0.17 0.204 East Bernard, Texas Region 6

head,

trimmed 100

OD 0.156 (0.176)

1

1 3 3 7 7 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.016

0.018 0.029 0.027 0.031 0.050 0.053

0.042 0.108 0.101 0.158 0.110 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.099

0.09 0.167 0.158 0.219 0.19 Fresno, California Region 10 Cabbage,

field head 100

OD 0.153 (0.172) 1

1 3 3 7 7 0.059

0.058 0.078 0.115 0.052 0.060 0.029

0.028 0.029 0.037 0.029 0.031 0.014

0.016 0.015 0.020 0.025 0.026 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.122

0.122 0.142 0.192 0.126 0.137

### - 394 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Trial ID (City, State/Year) Commodity

or Matrix Total

Rate (lb a.i./A) (kg a.i./ha) PHI

(days) BYI

08330 (ppm) BYI

08330- enol (ppm) BYI 08330-

ketohydroxy (ppm) BYI

08330-

monohydroxy (ppm) BYI

08330-enolGlc (ppm) Total

Residues of BYI 08330 (ppm)

head, trimmed 1 1 3 3 7 7 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.013

0.012 0.024 <0.010 0.012 0.014 0.017

0.010 0.024 0.020 0.025 0.020 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.06

0.052 0.078 0.06 0.067 0.064



### LEAFY BRASSICA

Trial ID (City, State/Year) Commodity

or Matrix Total

Rate (lb a.i./A) (kg a.i./ha) PHI

(days) BYI

08330 (ppm) BYI

08330- enol (ppm) BYI 08330-

ketohydroxy (ppm) BYI

08330-

monohydroxy (ppm) BYI

08330-enolGlc (ppm) Total

Residues of BYI 08330 (ppm)

Tifton, Georgia Region 2 Mustard

Greens 100

OD 0.157 (0.176) 1

1 3 3 7 7 0.176

0.159 0.049 0.058 <0.010 <0.01 1.098

1.091 0.348 0.357 0.091 0.097 0.338

0.354 0.177 0.206 0.051 0.050 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.111

0.076 0.104 0.091 0.096 0.078 1.733

1.69 0.688 0.722 0.258 0.245

Frenchtown, New Jersey Region 2 Mustard

Greens 100

OD 0.164

(0.184) 1

1 3 3 7 7 1.743

1.549 0.960 1.126 0.146 0.117 3.216

3.167 2.036 2.447 1.197 1.204 0.503

0.487 0.428 0.539 0.257 0.275 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.018

0.013 0.017 0.031 0.053 0.048 5.49

5.226 3.451 4.153 1.663 1.654

Oviedo, Florida Region 3 Mustard

Greens 100

OD 0.153 (0.171) 1

1 3 3 7 7 0.683

0.668 0.119 0.175 0.023 0.011 2.295

2.292 1.472 1.428 0.694 0.593 0.692

0.800 0.499 0.515 0.327 0.323 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.262

0.245 0.394 0.300 0.245 0.347 3.942

4.015 2.494 2.428 1.299 1.284

Leland, Mississippi Region 3 Mustard

Greens 0 0 1 1 1 3 3 7 7 10 10 0.023

0.011 0.026 <0.010 1.714 1.917 2.675 2.422 3.331 1.439 1.386 0.081

0.067 0.045 0.048 2.031 1.621 1.524 1.332 2.032 0.977 1.398 0.560

0.706 0.668 0.628 0.616 0.401 0.307 0.094 0.133 0.083 0.092 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 0.041

0.035 0.067 0.075 0.097 0.127 0.102 0.125 0.092 0.059 0.085 0.715

0.829 0.816 0.771 *4.468 4.076 4.618 3.983 5.598 2.568 2.971 Washed cooked greens 1 <0.010 0.399 0.014 <0.010 <0.010 0.443

Washed greens 100

OD 0.156

(0.175)

1 0.246 0.474 0.575 <0.010 0.070 1.375

### - 395 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

Trial ID (City, State/Year) Commodity

or Matrix Total

Rate (lb a.i./A) (kg a.i./ha) PHI

(days) BYI

08330 (ppm) BYI

08330- enol (ppm) BYI 08330-

ketohydroxy (ppm) BYI

08330-

monohydroxy (ppm) BYI

08330-enolGlc (ppm) Total

Residues of BYI 08330 (ppm)

Seymour, Illinois Region 5 Mustard

Greens 100

OD 0.155

(0.174) 1

1 3 3 7 7 0.058

0.056 0.030 0.041 <0.010 0.011 0.511

0.553 0.367 0.534 0.196 0.228 0.190

0.189 0.209 0.213 0.117 0.106 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.036

0.039 0.071 0.068 0.059 0.043 0.805

0.847 0.687 0.866 0.392 0.398 Seymour, Illinois Region 5 Mustard

Greens 240

SC 0.155 (0.174) 1

1 3 3 7 7 0.042

0.041 0.025 0.023 <0.010 <0.010 0.591

0.540 0.458 0.461 0.190 0.212 0.195

0.168 0.186 0.215 0.102 0.106 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.023

0.025 0.041 0.039 0.039 0.039 0.861

0.784 0.72 0.748 0.351 0.377

East Bernard, Texas Region 6 Mustard

Greens 100

OD 0.158 (0.177) 1

1 3 3 7 7 0.369

0.428 0.148 0.160 0.150 0.088 0.334

0.210 1.405 1.332 1.200 1.149 0.493

0.534 0.403 0.337 0.144 0.209 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.039

0.041 0.039 0.038 0.030 0.031 1.245

1.223 2.005 1.877 1.534 1.487

Fresno, California Region 10 Mustard

Greens 100

OD 0.156 (0.175) 1

1 3 3 7 7 1.160

1.240 0.861 0.731 0.042 0.030 1.405

1.332 1.200 1.149 0.386 0.361 0.758

0.754 0.669 0.558 0.176 0.201 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.045

0.042 0.095 0.072 0.032 0.034 3.378

3.378 2.835 2.52 0.646 0.636

Fresno, California Region 10 Mustard

Greens 240

SC 0.157 (0.176) 1

1 3 3 7 7 1.719

1.678 0.741 0.915 0.029 0.026 1.565

1.594 0.928 1.138 0.339 0.335 1.010

1.140 0.615 0.767 0.191 0.198 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.035

0.038 0.039 0.045 0.024 0.021 4.339

4.46 2.333 2.875 0.593 0.59

Oxnard, California Region 10 Mustard

Greens 100

OD 0.159 (0.178) 1

1 3 3 7 7 2.029

1.985 1.750 1.546 0.170 0.148 0.930

1.040 0.891 0.861 0.449 0.518 1.292

1.146 0.840 0.854 0.327 0.325 <0.010

<0.010 <0.010 <0.010 <0.010 <0.010 0.026

0.024 0.031 0.028 0.019 0.020 4.287

4.205 3.522 3.299 0.975 1.021

### - 396 -

Spirotetramat – Volume 3, Annex B.7 Residue data April 2008

HOPS Residues (ppm) Study Trial No. Trial SubID City, State Year EP 1 PHI 2 (days ) BYI 08330 BYI

08330 cis-enol BYI

08330cis-ketohydroxy BYI

08330

monohydroxy BYI

08330enolglucosid

e Total BYI08330 calc. 3

RAFNY022 FN229-05H Greenleaf, Idaho 2005 150 OD 7 7 14 14 4.242

3.946 2.916 3.131 0.639

0.501 0.494 0.483 0.202

0.156 0.232 0.270 <0.10

<0.10 <0.10 <0.10 0.637

0.456 0.689 0.792 5.82

5.159 4.431 4.776

RAFNY022 FN230-05H Woodburn, Oregon 2005 150 OD 8 8 14 14 4.083

3.676 3.634 3.554 0.744

0.705 0.684 0.515 0.220

0.206 0.298 0.196 <0.10

<0.10 <0.10 <0.10 0.663

0.488 0.652 0.594 5.81

5.175 5.368 4.959

RAFNY022 FN231-05H FN231-05H-A Yakima, Washington 2005 150 OD 7 7 14 14 1.590

1.430 1.806 1.623 0.236

0.451 0.377 0.344 <0.10

<0.10 <0.10 <0.10 <0.10

<0.10 <0.10 <0.10 0.138

0.355 0.395 0.404 2.164

2.436 2.778 2.571