Flonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 1 of 28 **UNITED STA**

**TES ENVIRONMENTA L PROTECTION A** **GENCY WA** **SHINGTON, D.C. 20460 OFFICE OF**  **CHEMICAL SAFETY AND**  **POLLUTION PREVENTION MEMORANDUM**  **Date:** October 2, 2012 **SUBJECT: REVISED**  . **Flonicamid** . Petition for the Establishment of Permanent Tolerance s

and Registration for Use on Berry Lo w - Growing S ubgroup 13 - 07G, Cucumber for Greenhouse Use Only , and Rapeseed Sub - group 20A . Summary of Analy tical Chemistry

and Residue Data. **PC Code:** 128016 **DP Barcode:** D 396 902 **Decision No.:** 45 7726 **Registration No. :**  71512 - 10 , 71512 - 9 **Petition No.:** 1E7942 **Regulatory Action:** Section 3 Registration **Assessment Type: Single Chem** **ical Case No.:**  NA **T XR No.:**  NA **CAS No.:** 158062 - 67 - 0 **MRID No.:** See Table Below **40 CFR:** 180. 613 **FROM:** Amelia M. Acierto , Chemist

Risk Assessment Branch III (RAB3) Health Effects Division (HED ; 7509P) **THROUGH:** Stephen Funk , Senior Scientist

Risk Assessment Branch III (RAB3) Health Effects Division (HED ; 7509P ) **TO:** Barbara Madden/Sydney Jackson , RM #5 Risk Integration, Minor Use and Emergency Response Branch ( RIMUERB) Registration Division (7505P) Note: The DER for greenhouse use on cucumber was originally pr epared by the Pest Management Regulatory Agency (PMRA) of Health Canada and DERs for berry and canola were originally prepared under contract by Versar, Inc. (6850 Versar Center, Springfield, VA 22151; submitte d 4/ 3 /12). The DERs hav e been reviewed by HED and revised to reflect current Office of Pesticide Programs (OPP) policies. **MRID Sum ma**  **ry Table MRID No.**  **Study Type Com**  **me nts**  4 8 657101 860.15 00 New DER; 4 8657101 . der.doc Straw berry 4 8657102 860.1 5 00 New DER; 4 8657102 . der.doc Cuc umber 4 8657103 de.1 860.1 5 00 New DER; 4 8657103 . de.1. doc Canola 4 8657103 de . 2 860.1520 New DER; 4 8657103 . de.2. doc Canola processed foodFlonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 2 of 28 **Table of Contents** Executive Summary ................................ ................................ ................................ ........................ 3 Regulatory

Recommendations ................................ ................................ ................................ ........ 5 Pre - Registration Data Needs ................................ ................................ ................................ ....... 6 Condition - of

- Registrat ion Data Needs ................................ ................................ ........................ 6 Tolerance Considerations ................................ ................................ ................................ ................ 6 Analy tical Method ................................ ................................ ................................ ....................... 6 Recommended Tolerances ................................ ................................ ................................ .......... 6 International Harmonization ................................ ................................ ................................ ....... 7 Revisions to Petitioned - For Tolerances ................................ ................................ ...................... 7 Residue Profile ................................ ................................ ................................ ................................ 7 Residue Chemistry

Guidelines ................................ ................................ ................................ ........ 9 Directions for Use (860.1200) ................................ ................................ ................................ .... 9 Nature of the Residue in Plants and Livestock (860.1300) ................................ ....................... 10 Residue Analy

tical Methods (860.1340) ................................ ................................ .................. 11 Multiresidue Methods (860.1360) ................................ ................................ ............................ 11 Storage Stability

(860.1380) ................................ ................................ ................................ ..... 11 Food Handling (860.1460) ................................ ................................ ................................ ........ 12 Meat, Milk, Poultry , and Eggs (860.1480) ................................ ................................ ................ 12 Crop Field Trials (860.1500) ................................ ................................ ................................ .... 13 Strawberry ..................................................................................... ...... ..... 13 Cucumber.......................................................................................... ...... 1 5 Canola ................................ ................................ ................................ ................................ ... 16 Processed Food an d Feed ( 860.1520 ) ................................ ................................ ....................... 18 Canola ................................ ................................ ................................ ................................ ... 18 Confined Accumulation in Rotational Crops (860.1850) ................................ ......................... 20 Field Accumulation in Rotational Crops (860.1900) ................................ ................................ 20 Proposed Tolerances (860.1550) ................................ ................................ ............................... 20 Appendix I ................................ ................................ ................................ ................................ .... 23 International Residue Limits ................................ ................................ ................................ . 23 Appendix II ................................ ................................ ................................ ................................ ... 24 Tolerance Assessment Calculations ................................ ................................ .......................... 24 Berry , L ow growing, Subgroup 13 - 07G ................................ ................................ ............... 24 Cucumber (Greenhouse , Foliar) ................................ ................................ ............................ 24 Cucumber (Greenhouse, Chemigation)............................................................ 2 4 Rapeseed, Subgroup 20A ................................ ................................ ................................ ...... 25Flonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 3 of 28 **Executive Summary** Flonicamid is a systemic insecticide that immediately suppresses the feeding of sucking insect s on plants . From its chemical structure (including the nicotinic acid structure) , it would be expected to exhibit the same mode of action as similarly structured neo - nicotinoid pesticides. However, flonicamid has not been found to activate acety lcholine esterase (OP's and carbamates), or nicotinic acetylcholine receptors (neo - nicotinoids). Flonicamid has been described as a new chemistry (cyanomethyl trifluoromethyl nicotinamide) with a novel (but undefined) mode of action, different from other commerci ally available products. The Interregional Research Project No. 4 (IR - 4) has submitted crop field trial and greenhouse data generated during 2008 and 2009 growing season fro m the North American Free Trade Agreement (NAFTA) Growing Zones in support of th e petition for the establishment of permanent tolerances for the combined residues of flonicamid [N - (cyanomethyl) - 4 - trifluoromethylnicotinamide] and its metabolites TFNA (4 - trifluoromethylnicotinic acid), TFNA AM (4 - trifluoromethylnicotinamide), and TFNG [N - (4 - trifluoromethylnicotinoyl)glycine], in or on the following raw agricultural commodities (RACs): Berry low - growing subgroup 13 - 07G ....... . .... ... 1.4 ppm Cucumber * .............................. ... ...... ......1.3 ppm Rapeseed subgroup 20A ..................... . ... .......1.5 ppm * To in crease tolerance on cucumber for greenhouse use only . The petitioner proposes Section 3 registration of Beleaf TM 50SG (EPA Reg. No. 71512 - 10) and Flonicamid 50WG (EPA Reg. No. 71512 - 9 ) for use on the berry subgroup 13 - 07G, cucumber for greenhouse use, and the rapeseed subgroup 20A. Beleaf TM 50SG and Flonicamid 50WG are 50% water soluble granule (SG) formulation s of flonicamid ( contain ing 0.5 pound active ingredient per pound of formulated product) . The end - use product s can be applied with ground, aerial and c hemi gation equipment at the total rate of 0.267 - 0.269 lb ai/acre (equivalent rate calculated /plant for greenhouse use). A non - ionic surfactant w as used in the crop trials except for canola and for greenhouse cucumber treated by chem i gation. The propo sed pre - harvest interval s (PHI s) range from 0 - days for strawberry and cucumber to 6 - 8 days for canola. T olerances are established for residues of flonicamid under 40 CFR § 180. 613(a)(1) on various raw agricultural commodities (RAC s ) at levels ranging from 0.2 ppm on fruit, pome, group 11 and vegetable, tuberous and corm, subgroup 1C to 16.0 ppm on turnip greens; Brassica leafy greens subgroup 5 B; and raddish, tops. Tolerance on cucumber is currently included in the v egetable, cucurbit, group 9 at 0.40 ppm. T olerances have also been established under § 180. 613(a)(2) on livestock commodities including egg and milk at levels ranging from 0.03 ppm on fat of cattle, goat, horse, poultry, and sheep to 0.08 ppm o n meat by products of cattle, g oat, horse, poultry , and sheep.Flonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 4 of 28 The nature of the residue in plants and livestock is adequately understood for purposes of this petition . The metabolism of flonicamid in plant and livestock are identical. T he main pathway of metabolism involves hydrolysis of the cyano and am ide func tional groups in the molecule. The residues of concern in plants for the tolerance expression and risk assessment are flonicamid, TFNA, TFNA - AM and TFNG (D290386, A.M. Acierto, 4/22/2005) . The HED’s RARC (RARC Sec. 3.0 , 4/20 /05) has determined th at the residues of concern in livestock commodities for the tolerance expression and risk assessment are flonicamid , TFNA and TFNA - AM. An a dequate enforcement method is av ailable which us es high p erformance liquid chromatography

with tandem mass spectrome tric detection (L C/MS/MS) adapted from FMC No. P - 3561M . The method has been used for data collection and enforcement for plant commodities. The method determines flonicamid and its metab olites TFNA, TFNA - AM and T FNG and has been sufficiently validated in five diverse crops. A number of minor modifications to the method were made for the petitioned crops including changes in clean - up procedures, reagents, and sample sizes. An L C - MS method similar to the L C/MS/MS method was used for cucumber. Method valid ation and concurrent recoveries in strawberry, cucumber and canola were conducted using untreated control samples fortified separately with flonicamid and its metabolites at 0.02, 0.20 and 2.0 ppm. The fortification levels were adequate to bracket expecte d residue levels in the strawberry and cucumber. The quantifiable residues were converted to parent equivalents by the study reviewer using molecular weight conversion factors of 1.20, 1.21, and 0.92 for TFNA, TFNA - AM, and TFNG, respectively . The L OQ (de termined as the LLM V) was 0.02 ppm for each analy te and the L OD was calculated as 1/3 the LOQ. Incanola, poor method validation recoveries and poor concurrent recoveries were reported using the HPL C/MS/MS method for each analy te at the 0.02 ppm fortification level. T he petitioner noted that this is caused by ion suppression due to matrix interference. HED recommends rais ing the lim i t of quantitation (L OQ) for each analy te to 0.2 ppm or about 0.9 ppm for the combined residues of flonicamid and its metabol ites, calculated as flonicamid (ChemSAC Minutes, 4/2/12). Three enforcement methods are used for livestock commodities: an LC /MS/MS method RCC No. 844743 (for the determination of residues in eggs and livestock tissues), L C/MS method RCC No. 842993 (for determin ation of residues in milk) and L C/MS/MS method FMC No. P 3580 , which includes an acid hydrolysis step ( for determin ation of residues in meat and meat products (muscle, kidney and liver) of cattle, goat, hog, horse, and sheep . The multi - residue methods requirement has been fulfilled. Flonicamid and TFNA - AM were completely

recovered using Protocol D (with no cleanup) but were not recovered using Protocol s E and F. Metabolites TFNA and TFNG were not recovered using Protocol s B, D, E and F. Avai lable storage stability data demonstrate that flonicamid and its metabolites TFNA, TFNA AM, and TFNG are relatively stable in/on oil seed, non - oily grain, root and tuber crops, leafy vegetables, and fruiting vegetable s in frozen storage for ~23 months. St orage stability data demonstrate that processed commodities are also stable for ~23 months. The current storage stability data demonstrate that residues of flonicamid, TFNA, TFNA - AM, and TFNG are stable in/on the RAC samples of berry , cucumber and canola stored frozen for up to 460, 336 and 735 days , respectively . The available data on the five diverse crops (oil seed, non - oily grain, root andFlonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 5 of 28 tuber crop, leafy

vegetables, and fruiting vegetables) are adequat e to support the storage conditions and duratio ns of the RAC samples from the submitted field trials . Adequate field trial data were submitted supporting the use of the flonicamid 50SG formulation on the proposed crop/crop groups. An adequate number of field trials were conducted on the required representative crops in the appropriate geographic regions . The crop field trial data reflect the proposed multiple application rates and pre - harvest interval s (PHI s ). The Organization of Economic Cooperation and Development (OECD) sp r eadsheet calculation procedure was used to determine appropriate tolerance levels. T he proposed tolerance for berry , low - growing , subgroup 13 - 07G is 1.4 ppm ; the proposed tolerance for greenhouse cucumber is 1.3 ppm . Based on the OECD spreadsheet calculation procedure , the prop osed tolerances for berry and cucumber as a member of the cucurbit vegetable group should be raised to 1.5 ppm . Therefore, a revised Section F is required to reflect this determination. The recommended tolerance of 1.5 ppm will replace the existing tolerance of 0.40 ppm for the cucurbit vegetable group 9 under 40 CFR § 1 80.613 (a)(1) . The proposed tolerance of 1.5 ppm for rapeseed is appropriate. Field trial decline studies demonstrate that the combined residues of flonicamid and its metabolites in strawberry decline with increasing pre - harvest intervals. Residue decline was observed in greenhouse grown cucumber treated by foliar spray

but not in crops treated by chemigation where the residues increased from the 0 - to 7 - day PHI s . No decline study

was reported for canola. Adequate processing studies in/ on canola are available. The processing data indicate that the combined residues of flonicamid, TFNG, TFNA, and TFNA - AM do not concentrate in canola meal and canola oil (each have 0.27x average processing factor). The reported processing factors do not exceed the theoretical concentration factor of 1.0x for canola meal and 3.0x fo r canola oil ( OCSPP § 860.1520, Table 3). Based on these results , the tolerance s for livestock commodities will not change. No new rotational crop data were submitted and none are required w ith the use of flonicamid on rapeseed, cucumber and berry ( OCSPP 860.1850). There are currently

no Codex or Canadian maximum residue limits (MRL s) established for residues of flonicamid i n crop or livestock commodities. The analy tical standard s for flonicamid, and its metabolites ( TFNA, TFNA - AM and TENG) are available at the EPA National Pesticide Standards Repository with expiration dates from 2014 - 2016 . **Regula tory Recommendations**  Provided the revision s to the Section B/label and Section F are made as requested below (in the Pre -Registration Data Needs section), the available residue chemistry data are adequate to support registration of the crop/crop group co mmodities requested by the petitioner at the tolerance levels recommended in Table 1 below (in the Recommended Tolerances section).Flonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 6 of 28 **Pre -**  **Registration Data Needs** The submitted la

bel s for BeleafTM 50SG Insecticide and Flonicamid 50WG have a restriction prohibiting greenhouse use. The label s should be revised to : “Do not use this product in greenhouses , except on cucumbers ”. The registrant needs to submit a revised section F in which the recommended tolerances and commodity

definitions listed in Table 1 are proposed. **Condition -**  **of**

**- Registration Data Needs**  No residue chemistry

conditional registration data needs are associated with this tolerance petition. **Tolerance Considerations Analytical Method**  Adequate enforcement methods are available to enforce the proposed tolerances for flonicamid and the major metabolites in plants and livestock. The proposed method for plants uses LC /MS/MS (FMC No. P - 3561M) to determine the residues of flonicamid and its major metabolites, TFNA - AM (4 - trifluoromethylnicotinamide ), TFNA (4 - trifluoromethylnicotinic acid), and TFNG [N - (4 - trifluoromethylnicotinoyl)glycine]. The reported LOQ was 0.0 2 ppm and the reported LOD was calculated as 1/3 the L OQ. This L OQ was demonstrated for cucumber and strawberry , but not for canola. Based on the poor results in the method validation and concurrent recoveries for canola at 0.02 ppm fortifications per analy t e , it is required to raise the LOQ to 0.2 ppm per each analy te ( 3/1 4 / 12) . Recoveries were consistently acceptable at the 0.2 ppm p er analy

te fortification level. **Recommended Tolerances** Tolerances should be established in 40 CFR §180. 61 3 with the following tolerance expression, as per the Steve Knizner memo dated 5/27/09: Tolerances are established for the residues of the insectic ide flonicamid including its metabolites and degradates, in or on the commodities in the following table. Compliance with the tolerance levels specified in the following table is to be determined by measuring only the sum of flonicamid [N - (cyanomethyl) - 4 - (trifluoromethyl) - 3 - py ridinecarboxamide] and its metabolites TFNA (4 - trifluoromethylnicotinic acid), TFNA - AM (4 - trifluoromethylnicotinamide), and TFNG [N - (4 - trifluoromethylnicotinoyl)glycine], calculated as the stoichiometric equivalent of flonicamid , in o r on the following commodities. HED recommends for establishment of tolerances on the commodities in Table 1 using the same tolerance expression as above at the tolerance levels recommended in Table 1 below :Flonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 7 of 28 **Table 1. Tolerance Sum ma**  **ry for Flonicam id**  **Com mo**  **dity Established/Proposed**  **Tolerance (ppm** **) Recom**  **me nded** 

**Tolerance (ppm** **) Com**  **me nts (correct** 

**com mo**  **dity definition)** Berry, low

growing, subgroup 13 - 07G 1.4 1 . 5 1 Cucumber for greenhouse use only 9 1.3 1.5 2 Vegetable, cucurbit, group 9 Rapeseed subgroup 20A 1.5 1.5 3 1 The representative commodity for the berry, low growing, subgroup 13 - 07G is strawberry. The Organization of Economic Coordination and Development ( OECD ) spreadsheet calculation procedure gave a value of 1.5 ppm for strawberry. 2 A toleran ce wa s established on cucumber at 0.4 ppm (as a member of the cucurbit vegetable group 9) . The current petition is to increase the tolerance to 1.3 ppm for cucumber grow n in greenhouse only. The OECD spreadsheet calculation procedure gave a value of 1.5 ppm for cucumber grown in the greenhouse treated at the proposed label rate by foliar spray. The OECD spreadsheet calculation procedure gave a value of 0.7 ppm for cucumber treated by chemigation . This tolerance value and the existing tolerance of 0.40 pp m in 40 CFR §180.613 will be covered under the foliar spray treatment in greenhouse . 3 The representative commodity for the rapeseed , subgroup 20A is canola. The OECD spreadsheet calculation procedure gave a value of 1.5 ppm for canola . No tolerances are required for the processed commoditie s of canola based on the demonstrated processing factor of <0.27x for each canola meal and canola oil. The maximum theoretical concentration factors for canola meal and canola oil are 1.9x and 3.0x, respectively ( O CSPP 860.1520, Table 3). **International Harmonization** There are no Codex or Canadian maximum residue limits (MRL s) on the proposed crops. **Revisions to Petitioned -**  **For Tolerances** Based on the OECD spreadsheet calculation procedure, HED recommends incre asing the proposed tolerance from 1. 4 ppm to 1.5 ppm for ber ry , low growing , subgroup 13 - 07G and from 1.3 ppm to 1.5 ppm for greenhouse grown cucumber (as a member of the cucurbit vegetable group) . **Residue Profile** The chemical structure and nomenclature of flonicamid and its metabolites TFNA, TFNA - AM, and TFNG, and the physicochemical properties of the technical grade of flonicamid are presented in Tables 2 and 3 .Flonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 8 of 28 **TABLE 2 .**  **Test Com pound Nom**  **enclature.** Compound

N CF 3 N

H O CN Common name Flonicamid Company experimental name IKI - 220 IUPAC name N - cyanomethyl - 4 - (trifluoromethyl)nicotinamide CAS name N - (cyanomethyl) - 4 - (trifluoromethyl) - 3 - pyridinecarboxamide CAS registry number 158062 - 67 - 0 End - use product (EP) 50% SG formulation; Beleaf 50 SG (EPA Reg. No. 71512 - 10) Compound

N CF 3 O H O

Common name TFNA Chemical name 4 - trifluoromethylnicotinic acid Compound

N CF 3 N H

2 O

Common name TFNA - AM Chemical name 4 - trifluoromethylnicotinamide Compound

N CF 3 N

H O O H

O Common name TFNG Chemical name N - (4 - trifluoromethylnicotinoyl)glycine **TABLE 3 .**  **Physi cochem** **ical Properties of the Technical Grade Test Com pound Flonicam** **id. Param**  **eter Value**  **Reference 1**  Melting point 157.5  C MRID 45854601 pH 4.5 (25  C) Density 1.531 (20  C) Water solubility 5.2 g/L (20  C) Solvent solubility Solvent g/100 mL (20  C) acetone 17.32 acetonitrile 12.04 dichloromethane 0.40 ethyl acetate 3.57 hexane 0.00003 isopropyl alcohol 1.46 methanol 9.76 n - octanol 0.26 toluene 0.03 MRID 45656705Flonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 9 of 28 **TABLE 3 .**  **Physi cochem** **ical Properties of the Technical Grade Test Com pound Flonicam** **id. Param**  **eter Value**  **Reference 1**  Vapor pressure 9.43 x 10 - 7 Pa (20  C) 2.55 x 10 - 6 Pa (25  C) MRID 45854601 Dissociat ion constant, pKa 11.60 ± 0.03 (20 ± 1  C) MRID 45656705 Octanol/water partition coefficient, Log(KOW) 1.9 (Log P OW = 0.3) (29.8  C) MRID 45854601 UV/visible absorption spectrum Acidic and neutral aqueous solutions exhibited similar spectra with an absor

ption maximum near 265 nm and a molar absorptivity of 3,900 L/cm mol. A basic solution exhibited two absorption peaks. The peak observed in acidic and neutral solutions was present at a slightly longer wavelength, 270 nm, with an absorptivity of 4,200 L/cm mol. The second peak had an absorption maxima at 204 nm with an absorptivity of 13,200 L/cm mol. 1 RD Memo, DP# 285457, 9/30/2003, S. Mathur **Residue Chemistry Guidelines Directions for Use**  **(860.1200 )**  The petitioner ha s submitted amended label s for a 50 SG formulation ( Beleaf 50SG Insecticide , EPA Reg. No. 71512 - 10 ) and for the 50WG formulation (Flonicamid 50WG, EPA Reg. No. 71512 - 9) . A summary

of the proposed use patterns on berry , low growing ( subgroup 13 - 07G ) , greenhouse grown cucumber s , and rapesee d (subgroup 20B) is detailed in Table 4 . **Table 4**  **. Sum ma**  **ry of Directions for Use of Flonicam** **id Application,**  **Timing, Type and**  **Equipment Formulation** 

**(EPA Reg. No**  **s .)**  **. App.**  **Rate**

**(lb ai/A) [fl oz /A]**  **Max. No.**

**App. per Season**  **RTI**

**(days) Max.** 

**Seasonal App.**  **Rat e**  **(lb ai/A) [fl oz /A]**  **PHI**

**(days) Use Directions and other Limitations**  Berry, low growing, subgroup 13 - 07G [Bearberry, bilberry, blueberry, lowbush, cloudberry, cranberry, lingonberry, muntries partridgeberry, strawberry, cultivars, varieties, and/or hyb rids of these] 1

. F oliar spray ground or air Beleaf 50SG

( EPA Reg . No . 71512 - 1 0 ) or Flonicamid 50WG (EPA Reg. No. 71512 - 9) 0.089

[ 2.8 ] 3 7 0.267 [ 8.4 ] 0 Apply whe n Aphids or L ygus first appear in the field and before populations reach high levels. Flonic amid will stop Aphids or L

ygus feeding rapidly but it may take several days to see reduction in Aphids or L ygus numbers. Reapply when new insects are detected. Two sequential applications of flonicamid result in better Aphids or L

ygus control than a singl e application. Do not make more than 2 applications of flonicamid without rotating to an insecticide with a different mode of action. Greenhouse Cucumber sFlonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 10 of 28 **Table 4**  **. Sum ma**  **ry of Directions for Use of Flonicam** **id Application,**  **Timing, Type and**  **Equipment Formulation** 

**(EPA Reg. No**  **s .)**  **. App.**  **Rate**

**(lb ai/A) [fl oz /A]**  **Max. No.**

**App. per Season**  **RTI**

**(days) Max.** 

**Seasonal App.**  **Rat e**  **(lb ai/A) [fl oz /A]**  **PHI**

**(days) Use Directions and other Limitations** 

Foliar directed Beleaf 50SG

( EPA Reg . No . 71512 - 10 ) or Flonicamid 50WG (EPA Reg. No. 71512 - 9) 0. 089

[ 2.8 ] 2 7 4.28 oz/A or 0.1 oz per 1000 ft2 0 1) For Aphids Plant Bugs. Begin applications before

population s begin to build and before damage is evident, according to local pest management guidelines. Use LOWER RATE for building populations and HI GHE R RATE for greater populations and/or dense foliage. Rapidly growing plants may need retreatment. Check plants often and retreat as ne c essary

to maintain population below damaging levels. 2) For Greenhouse White f ly . Apply whe n adult whiteflies first appe ar . Do not allow population to increase unchecke d before making the first application. Application provides SUPPRESSION only. Apply in combination with other effective products for control. Check plants often and retreat as necessary to maintain population below damaging levels. Chemigation (to soil or growth media) Bel eaf 50SG

( EPA Reg . No . 71512 - 10 ) or Flonicamid 50WG (EPA Reg. No. 71512 - 9) 0.089

[ 2.8 ] 2 7 4.28 oz/A or 2.8 g/1000 ft2 0 Begin applications before population s begin to build

and before damage is evident according to local pest managem ent guidelines. Apply using a drench by hand, drip irrigation or with motorized calibrated irrigation equip ment to the base of the plants. 2 Rapeseed Subgroup 20 A [Borage, crambe, cuphea, echium, flax seed, gold of pleasure, hare’s ear mustard, lesquerella, lunaria, meadowfoam , milkweed, mustard seed, oil raddish, poppy seed, rapeseed, sesame, sweet rocket, cultivars varieties, and/or hybrids of these ]. Foliar spray ground or air Beleaf 50SG

( EPA Reg . No . 71512 - 10 ) or Flonicamid 50WG (EPA Reg. No. 71512 - 9) 0.089

[ 2.8 ] 3 7 0.26 7 [ 8.4 ] 7 Apply whe n Aphids or L ygus first appear in the field and before populations reach high levels. Flonicamid will stop Aphids or L

ygus feeding rapidly but it may take several days to see reduction in Aphids or L ygus numbers. Reapply when new insec ts are detected. Two sequential applications result in better Aphids or Lygus control than a single application. Do not make more than 2 applications of flonicamid without rotating to an insecticide with a different mode of action. 3 1 Spray adjuvants may improve coverage but do not use binder or sticker - type surfactants. Only use adjuvants known to be safe on strawberries. 2 Use a minimum of 25 gal/1000 plants but do not exceed the holding capacity of soil or growth media. Do not apply more than 4.28 oz/A (0.44 oz/10 00 plants based on 1 plant/4.5 ft2 or 9712 plants/A) of flonicamid per application. 3 Spray adjuvants may

improve coverage but do not use binder or sticker - type surfactants. Only use adjuvants known to be safe on canola The submitted la

bel s f or BeleafTM 50SG Insecticide and Flonicamid 50WG have a restriction for greenhouse use . The label s should be revised to change the statement “Do not use this product in greenhouses” to “Do not use this product in greenhouses , except for cucumber” . Conclusions . The submitted label s (EPA Reg. No s . 71512 - 10 and 71512 - 9 ) are adequate to allow evaluation of the residue data relative to the proposed use. R evised label s are required to delete the restriction for greenhouse use for cucumber . **Nature of the Resi due**  **in Plants and Livestock (860.1300**  **)** No new metabolism data were submitted in support of this petition and none are required. The nature of the residue in plants and livestock is adequately understood . Based on the metabolism studies conducted in plants, the major metabolic pathway of flonicamid in plants involves hydrolysis of the cyano ( - CN) and amide ( - CONH) functional groups and ring hydroxylation.Flonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 11 of 28 The residues of concern in plants for tolerance and risk assessment are flonicamid and its metabolit es TFNA, TFNA - AM, and TFNG (D290386, A.M. Acierto , 4/22/2005 ) . In livestock commodities, HED has determined that the residues of concern for the tolerance expression and risk assessment are flonicamid, TFNA and TFNA - AM (HED/RARC Sec. 3.0, 4/20/05). **Resid ue Analytical Methods**  **(860.1340 )**  The method entitled “Analy tical Methodology

for IKI - 220 (F1785) and its Major Metabolites in/on Peach, Potato Tuber, and Wheat Straw” (FMC No. P - 3561M) was used with some modifications to determine residues of flonicamid and its metabolites TFNA - AM (4 - trifluoromethylnicotinamide), TFNA (4 - trifluoromethylnicotinic acid), and TFNG [N - (4 - trifluoromethylnicotinoyl)glycine] in/on strawberry and canola. Cucumber fruit samples were analy zed for the residues of flonicamid and the three major metabolites, using a liquid chromatography

with mass spectroscopic detection (L C - MS) working method entitled “Residue Analysis of Flonicamid, TFNA, TFNG, TFNA - AM by L C/MS, Version #3”. A number of minor modifications to the methods were made, including changes in clean - up procedures, reagents, and sample sizes. To calculate the total of all flonicamid, TFNA, TFNA - AM and TFNG residues (the residue definition in plant matrices), residues of the 3 metabolites above the lowest level of method val idation ( LLM V ) were converted to flonicamid equivalents (MW flonicamid = 229.17 g/mol) prior to summing using the following conversion factors: 1.2 for TFNA (MW = 191.11 g/mol) , 1.21 for TFNA - AM (MW = 190.12 g/mol); and, 0.92 for TFNG (MW = 248.2 g/mol). The LOQ (determined as the LLMV) was 0.02 ppm for each analy te , except in canola . For canola matrices, poor recoveries were obtained at the 0.02 ppm fortification for canola matrices. Satisfactory recoveries were obtained at a fortification level of 0. 2 ppm for each of the four analy tes. The limit of detection (L OD) was calculated as 1/3 the LOQ. **Multiresidue Methods (860.1360)**  The multi - residue method (MRM) data were reviewed previously and the testing data have been forwarded to FDA for inclusion i n PAM , Vol. I . The multi - residue methods requirement has been fulfilled. Flonicamid and TFNA - AM were completely recovered using Protocol D (with no cleanup) but were not recovered using Protocols E and F. Metabolites TFNA and TFNG were not recovered usi ng Protocols B, D, E and F. Flonicamid and its metabolites TFNA (4 - trifluoromethylnicotinic acid), TFNA - AM (4 - trifluoromethylnicotinamide), and TFNG [N - (4 - trifluoromethylnicotinoyl)glycine] were analy zed according to the FDA Multi - Residue Method Test guid elines in PAM , Vol. I(dated 1/94). Flonicamid and its metabolites were tested through Protocols A and C, and as a result of Protocol C testing, all compounds were tested through Protocols D and E. Based on the results of Protocol E testing, testing under Protocol F was not required. Since methylated TFNA and TFNG provided good response on at least one of the column/detector combinations outlined in Protocol C, additional testing was performed with these compounds under Protocol B. **Storage Stability (**  **860.1380)** DER Reference: 48657101 der doc (strawberry)

48657102 der.doc (cucumber)Flonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 12 of 28 48 65 7 103 d e 1 .doc (canola) 48657103 de 2 doc (canola processed commodities ) To support the sample storage intervals, untreated control RAC samples ( strawberry , cucumber and canola) and processed canola commodities ( canola meal and oil ) were fortified with each analy te ( flonicamid, TFNA, TFNA - AM and TFNG) at 0.2 ppm. The samples were extracted according to the method described under the analy tical method and stored at < - 15 to ~ - 21 o C from collection to extraction. Samples were analy zed within 1 - 14 days of extraction. The d ata demonstrate that residues of flonicamid, TFNA, TFNA - AM, and TFNG are stable in/on the RAC samples of strawberry , cucumber and canola stored frozen for up to 460, 336 and 735 days, respectively . The available data on five diverse crops (oil seed, non - oily grain, root and tuber crop, leafy

vegetables, and fruiting vegetables) are adequat e to support th e storage conditions and durations of the RAC samples for the subject petition. Results of the storage study are summarized in Table 5 . **TABLE 5. Stability of Flonicam** **id and its Metabolites in Strawberry , Cucum** **ber and Canola, Strawberry**  **Matrix Analyte**  **Spike Level**  **(ppm )**  **Storage interval**  **1 (days)**  **Fresh**

**Fortification Recoveries**  **(% )**  **Recovered Residues**

**(ppm )**  **Mean**

**Recovered Residues**  **(ppm )**  **Mean**

**Recovery (%**  **) Corrected** 

**% R**  **ecovery 2**  **,3** Strawberry Flonicamid 0.20 460 100 0.19, 0.20, 0.20 0.20 98 98

TFNA 0.20 460 90 0.17, 0.18, 0.18 0.18 88 98 TFNA - AM 0.20 460 80 0.16, 0.17, 0.17 0.17 83 104 TFNG 0.20 460 80 0.15, 0.16, 0.16 0.16 78 98 Cucumber Flonicamid 0.2 336 90, 90, 105 0.18, 0.18, 0.21 0.19 95 100

TFNA 0.2 336 80, 85, 95 0.16, 0.17, 0.19 0.17 85 102 TFNA - AM 0.2 336 80, 80, 90 0.16, 0.16, 0.18 0.17 85 104 TFNG 0.2 336 75, 80, 90 0.15, 0.16, 0.18 0.16 8 4 103 Canola (seed) Flonicamid 0.2 735 82 0.1 6 , 0.1 6 , 0.1 7 0.16 81 98

TFNA 0.2 735 74 0.12, 0.1 5, 0.16 0.14 72 97 TFNA - AM 0.2 735 82 0.16, 0.16, 0.16 0.16 81 99 TFNG 0.2 735 85 0.1 5 , 0.1 7 , 0.16 0.16 79 93 1 Interval from fortification to extraction. Samples were analyzed within 0 - 14 day s of extraction . 2 Corrected for mean recovery in freshly fortified samples. 3 Corrected by dividing the me an freezer storage stability recoveries by the co rresponding concurrent recovery . Conclusion s. The submitted storage stability data demonstrate that residues of flonicamid, TFNA, TFNA - AM, and TFNG are stable in/on the RAC samples of strawberry , cucumber and canola stored frozen for up to 460, 336 and 735 days, respectively . The available data on five diverse crops (oil seed, non - oily grain, root and tuber crop, leafy vegetables, and fruiting vegetables) support the storage conditions and durations o n strawberry , cucumber and canola. **Food Handling (860.1460)**  There are no proposed uses that are relevant to this guideline topic . **Meat, Milk, Poultry, and Eggs (860.1480)** Flonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 13 of 28 There are no proposed uses that are relevant to this guideline topic. **Crop Field T rials**  **( 860.1500**  **) Strawberry**  DER Reference : 48657101 The IR - 4 has submitted field trial data for flonicamid on strawberries . Eight field trials were conducted in the United States during the 2008 growing season in the North American Free Trade Agreement (NAFTA) Growing Zones 1 (NY; 1 trial), 2 (NC; 1 trial), 3 (FL ; 1 trial), 5 (WI ; 1 trial), 10 (CA; 3 trials), and 12 (OR; 1 trial). Two trials [CA*59 and CA*60 (Salinas, CA)] were conducted at the same location by the same field research director (FRD ) . The differences between the trials were: use of different tank mixes for all applications; a 60 - to 62 - day off - set in application dates; and use of different application equipment (in two of three applications ). HED has concluded that the differences are in sufficient to classify

the trials as two separate trials (ChemSAC , 11/2/2011) . The number of independent trials is seven. Each trial consisted of one untreated plot and one treated plot. At each trial location, the treated plot received three foli ar broadcast or directed applications of a 50% water soluble granule (SG) formulation of flonicamid (Beleaf 50 SG ) at 0.086 - 0.094 lb ai/A/application, for a total seasonal rate of 0.263 - 0.280 lb ai/A. Applications were made at the blooming to mature fruit stage with retreatment intervals (RTI) between 6 - to 8 - days , except at trials OR12 and FL24, where one application at each trial was made at an RTI of 10 - 11 days due to rain. Applications were made using ground equipment in spray volumes of 27 - 53 gal/A. Except for one trial, a nonionic surfactant (NI S) was added to the spray mixture for each of the applications . Samples were h arvested from all trials at a 0 - day pre - harvest interval (PHI) ; additional samples of strawberries were collected at PHI s of 3, 5, and 7 days from one trial (NC13) to assess residue decline . Samples were analy

zed for residues of flonicamid and metabolites TFNA, TFNA - AM, and TFNG using a high performance liquid chromatography method with tandem mass spectrometric detection (L C/MS /MS) adapted from FMC No. P - 3561M. The quantifiable residues of TFNA, TFNA - AM, and TFNG were convert ed to parent equivalents using molecular weight conversion factors of 1.20, 1.21, and 0.92, respectively (MW of flonicamid 229.17 ÷ MW of TFNA 191.11, MW o f TFNA - AM 190.12, or MW of TFNG 248.2 ) . The limit of quantitation (L OQ; determined as the lowest level of method validation, LLM V) was 0.02 ppm for each analy te. The method was adequate for data collection based on acceptable method validation and concur rent recovery data. The fortification levels used in method validation and concurrent method recovery were adequate to bracket expected residue levels. Concurrent recoveries and residues in the treated samples were not corrected for residues in controls. The LOD for each matrix was calculated by

multiplying the standard deviation of recovery measurements at the LLM V by the one - tailed t - statistic (confidence level not reported) for six to seven replicates, and the LOQ was defined as 3x the L OD. The calcu lated L OQs in strawberries were 0.0094, 0.0153, 0.0134, andFlonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 14 of 28 0.0104 ppm, respectively, for flonicamid, TFNA, TFNA - AM, and TFNG; corresponding calculated LOD values were 0.0031, 0.0051, 0.0045, and 0.0035 ppm . Following three foliar broadcast or directed a pplications of the 50% SG formulation of flonicamid at 0.263 - 0.280 lb ai/A, residues (and per trial averages) of flonicamid, metabolites TFNA, TFNA - AM, TFNG , and combined residues of the four analy tes, respectively , in/on strawberries harvested at a 0 - day PHIwere : 0.11 - 0.66 (0.13 - 0.54), <0.02 - 0.12 (<0.02 - 0.12), <0.02 (<0.02), <0.02 - 0.083 (<0.02 - 0.080), and <0.17 - <0.79 (<0.19 - <0.73) ppm . Data from the residue decline trial showed that residues of flonicamid and combined residues decreased in strawberrie s with increasing PHI s ; howeve r, residues of TFNA increased with increasing PHI s. Residue decline could not be assessed for TFNA - AM and TFNG because residues were below the LOQ in/on all samples. A summary

of residue data from the strawberry field trials is presented in Table 6. **TABLE 6 . Sum**  **ma ry of Residue Data from** **Strawberry Field Trials with Flonicam id.**  **Com modity**  **Analyte Total**  **Rate (lb ai/A)**  **PHI**

**(days) Residue Levels (ppm**  **flonicam id equivalents)**  **n Sam** **ple Min.**  **Sam ple**  **Max. LAFT**  **1 HAFT**  **1 Media**  **n Mea**  **n Std.** 

**Dev.** Strawberry, Berries with caps removed Flonicamid 0.263 - 0.280 0 7 0.11 0.66 0.13 0.54 0.34 0.34 0.16

TFNA <0.02 0.12 <0.02 0.12 0.052 0.051 0.035 TFNA - AM <0.02 <0.02 <0.02 <0.02 0.02 0.02 N/A TFNG <0.02 0.083 <0.02 0.080 0.026 0 .036 0.022 Combined2 <0.17 <0.79 <0.19 <0.73 0.41 0.45 0.20 1 LAFT: Lowest average fielt trial; HAFT: highest average field trial 2 Combined residues of flonicamid, TFNA, TFNA - AM, and TFNG Conclusion s. The submitted strawberry f ield trial data are adequate. Following three f oliar broadcast or directed applications of the 50% SG formulation of flonicamid at 0.263 - 0.280 lb ai/A, residues (and per trial averages) of flonicamid, metabolites TFNA, TFNA - AM, TFNG , and combined residues of the four metab olites, respectively, in/on strawberries harvested at a 0 - day PHIwere : 0.11 - 0.66, <0.02 - 0.12, <0.02, <0.02 - 0.083, and <0.17 - <0.79 ppm. Data from the residue decline trial showed that residues of flonicamid and total residues decreased in strawberries wi th increasing PHI s; however, residues of TFNA increased with increasing PHI s. Residue decline could not be assessed for TFNA and TFNG because residues were below the LOQ in/on all samples. An acceptable method was used for residue quantitation, and adequ ate data were submitted to support sample storage intervals and conditions.Flonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 15 of 28 **Cucumber** DER Reference : 4865710 2 Four greenhouse cucumber trials were conducted in zones 2 (1 trial each in MD and TN), 5 (1 trial in ON) and 9 (1 trial in CO) during 2008 an d 2009. Each trial site consisted of two treated plots and one untreated control plot. At one of the treated plots, two foliar ground applications of flonicamid (Beleaf 50SG insecticide) were applied 6 - 7 days apart at rates ranging from 0.129 - 0.147 lb a .i. /A (0.145 - 0.165 kg a.i./ha) per application for total rates of 0.262 - 0.291 lb a.i./A (0.294 - 0.326 kg a.i./ha) per season. A nonionic surfactant was included in the tank mix for the second foliar application at trial CO06 (Activator 90; 0.25% v/v) and in both foliar applications at trials TN04 (Co - Op; 0.25% v/v) and ON03 (Agral 90; 0.25% v/v). The second treated plot received two simulated chemigation applications of flonicamid to the rock wool substrate in which the cucumber plants were grown using a s yringe, 6 - 7 days apart. The rates (per acre [hectare]) determined using an average plant density of 2.4 plants per square meter, ranged from 0.130 - 0.134 lb a.i./A (0.146 - 0.150 kg a.i./ha) per application for total rates of 0.264 - 0.269 lb a.i./A (0.296 - 0.3 02 kg a.i./ha) per season. No adjuvants were included in any of the chemigation appli ed mixtures. Mature cucumber fruit samples were harvested from all treated plots on the day of the last application, after the foliar spray had dried (i . e . , 0 - day

PHI). At the ON03 trial, samples were harvested from both treated plots at additional PHI s of 3, 5, and 7 days to evaluate any residue decline . Cucumber fruit samples were analy zed for the combined residues of flonicamid and the three major metabolites, 4 - trif

luoromethylnicotinic acid (TFNA), 4 - trifluoromethylnicotinamid (TFNA - AM), and N

- (4 - trifluoro - methylnicotinoyl)glycine (TFNG), using a liquid chromatography

with mass spectroscopic detection (L C - MS) working method entitled “Residue Analysis of Flonicamid, TFNA, TFNG, TFNA - AM by L C/MS, Version #3”. This method is similar to the previously

reviewed reference method No. P - 3561 entitled “Analy tical Methodology

for IKI - 220 (F1785) and its Major Metabolites in/on Peach, Potato Tuber, and Wheat Straw, FMC Corp. P - 3561M”. The calculated limit of quantitation (L OQ) was 0.017 ppm for flonicamid, 0.0094 ppm for TFNA, 0.011 ppm for TFNA - AM, and 0.0081 ppm for TFNG. The limit of detection (L OD) was calculated to be 0.0056, 0.0031, 0.0036 and 0.0027 ppm for flonicamid, TFNA, TFNA - AM and TFNG, respectively . The LLM V for cucumber was determined to be 0.020 ppm for flonicamid and each of the metabolites. Based on acceptable method validation and concurrent recoveries within the range of 70 - 120%, the method is adequate for data gathering purposes in cucumber fruit matrices in this study . The maximum storage interval for treated cucumber samples was 329 days from harvest to extraction. All extracted samples were analy z ed within 14 days. Concurrent fre ezer storage stability tests conducted as part of the trial study demonstrated that residues of flonicamid, TFNA, TFNA - AM and TFNG are stable in cucumbers for up to 336 days of frozen storage, which adequately

covers the frozen storage interval for treated cucumber samples in this study . Incucumbers harvested at a 0 - day PHI , total residues of flonicamid and the TFNA, TFNA - AM and TFNG metabolites were <0.203 - <0.208 ppm following two foliar spray applications at total rates of 0.264 lb a.i./A (0.296 kg a. i./ha) without an adjuvant in the spray mixture and <0.106 - <0.775 ppm following two foliar applications at rates totaling 0.262 - 0.291 lb a.i./A (0.294 - 0.326 kg a.i./ha) including an adjuvant in one or both of the spray mixtures. In cucumbers harvested atFlonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 16 of 28 a 0 - day PHIfollowing two simulated chemigation applications to the growth medium at total rates of 0.264 - 0.269 lb a.i./A (0.296 - 0.302 kg a.i./ha), total residues were <0.079 - <0.341 ppm. Residue decline data indicated that following foliar applications, residues in cucumber fruit decreased with increasing PHI s from 0 - 7 days ; the residues increased slightly with increasing PHI s from 0 - 7 days in cucumber fruit following simulated chemigation applications to the growth medium. A summary

of residue data from the cucumber greenhouse trials is presented in Table 7. **TABLE 7**  **. Summary of Residue**  **Data from Greenhouse**  **Trials with Flonicam id.**  **Com modity**  **Analyte Total Rate**  **lb a i** **/A [kg ai/ha]**  **PHI**

**(days) Residue Levels**  **(ppm )**  **n Min.**  **Max. LAFT** * **HAFT*** **Median (STMdR)**  **Mean**

**(STMR) Std.** 

**Dev.** Foliar Cucumber fruit Flonicamid 0.262 - 0.291 [0.294 - 326 ] 0 4 <0. 046 0.69 0.054 0.54 0.101 0.2 0.23 - TFNA <0.02 0.034 <0.02 0.031 0.02 0.23 0.005 TFNA - AM <0.02 <0.02 <0.02 <0.02 0.02 0.02 0 TFNG <0.02 0.03 <0.0 2 0.028 0.02 0.23 0.004 Chemigation Cucumber fruit Flonicamid 0.264 - 0.269 [0.296 - 0.302] 0 4 0.012 0.2 0.013 0.2 0.112 0.11 0.073 TFNA <0.02 0.023 0.02 0.023 0.02 0.021 0.001 TFNA - AM <0.02 <0.02 <0.02 <0.02 0.02 0.02 0 TFNG <0.02 0.11 <0.02 0.11 0.02 0.043 0.04 *LAFT = Lowest average field trial; HAFT = Highest average field trial. C onclusion . The cucumber greenhouse trials are considered scientifically acceptable. In cucumbers harvested at a 0 - day

PHI, total residu es of flonicamid and the TFNA, TFNA - AM and TFNG metabolites were <0.203 - <0.208 ppm following two foliar spray with a djuvant added in both first and second spray mixtures , <0.106 - <0.775 ppm following two foliar applications with adjuvant added in the first spray mixtures. Total residues in cucumbers harvested at a 0 - day PHI following two simulated chemigation applications were <0.079 - <0.341 ppm. Residue decline was observed with increasing PHI in cucumber treated by foliar spray . The residues in the ch emigation treatment increased with increasing PHI from 0 to 7 days. **Canola** DER Reference: 48 657103 . de.1 The IR - 4 has submitted field trial data for flonicamid on canola . Nine field trials were conducted in the United States during the 2007 - 2008 growin g seasons in the North American Free Trade Agreement (NAFTA) Growing Zones 2 (NJ; 1 trial), 5 (SD; 3 trials), 7 (ND; 2 trials), and 11 (ID and WA; 3 trials). Two WA trials (WA05 and WA10) were conducted by different Principal Field Investigators (PFI s) at the same trial location; examination of the field trial records indicates that there areFlonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 17 of 28 sufficient differences between the trials, including a 372 - to 373 - day offset in application dates, for the trials to constitute separate trials for purposes of OCSPP 860.1500 data requirements. Three of the SD trials (SD02, SD03, and SD05) were conducted by the same PFI . Careful examination of the field trial records indicates that the only differences between trials SD02/SD03 were: use of different tank mixes for all applications, a ~7 - mile separation between the two trial locations, and a 1 - day off - set in application dates (application 1 only ). HED has concluded that the differences between the trials (SD02 and SD03) are insufficient to classify them as separate trials ; therefore, these trials constitute a single trial with replicate samples for purposes of OCSPP 860.1500 data requirements. Examination of the field trial records indicates that there are sufficient differences between trial s SD05 and SD02 /SD03, in cluding a 3 77 to 380 - day offset in application dates for this trial to constitute a separate trial. The adjustment in trial numbers results in a total of eight field trials , with two trials conducted in NAFTA Z o ne 5. Each trial consisted of one untreated plot and one treated plot. At each trial location, the treated plot received three foliar broadcast applications of a 50% water soluble granule (SG) formulation of flonicamid (Beleaf 50 SG ) at 0.085 - 0.092 lb ai/A/application, for a total seasonal rate of 0.261 - 0.272 lb ai/A. Applications were made at 6 - to 8 - day RTI s using ground equipment in spray volumes of 10 - 20 gal/A. No adjuvants were added to the spray mixtures at any

trial site . Samples of canola seed were harvested from all trials at a 6 - to 8 - day PHI) seed samples from four trial sites were dried in the field or greenhouse for 1 - 10 days prior to collection . Samples were analy

zed for residues of flonicamid and its metabo lites (TFNA, TFNA - AM, and TFNG) using the high performance liquid chromat ography with tandem mass spectrometric detection (LC/MS/MS) adapted from FMC No. P - 3561M. The limit of quantitation ( LOQ ; determined as the lowest level of method validation, LLM V) was 0.02 ppm for each analy te . Variable recoveries were obtained in metho d validation and concurrent method validation reflecting fortification with each analy te at 0.020, 0.20, and 2.0 ppm. Method validation recoveries were generally slightly low (flonicamid, TFNA, and TFNA - AM) to very low (TFNG) for all analy

tes at all forti fication levels except flonicamid at 2.0 ppm and TFNA - AM at 0.20 and 2.0 ppm, for which recoveries were acceptable (mean 78 - 84%). Concurrent recoveries for all analy tes were generally

acceptable at the 0.20 and 2.0 ppm fortification levels: mean recoveri es were 72 - 85% with standard deviations of 4 - 12% . However, low concurrent recoveries were obtained at 0.020 ppm: 53% for flonicamid, 68% for TFNA, 62% for TFNA - AM , and 41% for TFNG . The petitioner noted that the lower than expected recoveries were cause d by ion suppression due to matrix interference. Several approaches were taken to reduce the ion suppression, including additional cleanups and different elution programs, but the problem could not be eliminated. The ChemSAC reviewed the situation and co ncluded that the L OQ is 0.2 ppm for each analy

te in canola matrices (03/1 4 /2012). T he fortification levels used in method validation and concurrent method recovery were adequate to bracket expected residue levels. C oncurrent recoveries were corrected for residues in the controls; r esidues in the treated samples were not corrected for residues in controls. Q uantifiable residues of TFNA, TFNA - AM, and TFNG were converted to parent equivalents by the study reviewer u sing molecular weight conversion factors of 1.20, 1.21, and 0.92, respectively (MW of flonicamid 229.17 ÷ MW of TFNA 191.11, MW of TFNA - AM 190.12, or the MW of TFNG 248.2). Samples were stored frozen (< - 15 °C) from collection to analysis for 311 - 748 days (10.2 - 24.6 months). Samples were analy zed within 0 - 3 days of extraction . Storage stability data generatedFlonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 18 of 28 concurrently

with the field trial study

demonstrate that residues of flonicamid, TFNA, TFNA AM, and TFNG were stable in/on samples of canola stored frozen for up to 735 days (24.2 months) . Residue decline data on canola were not submitted. Since sufficient data have been reported on residue decline of residues in a variety of crops, further study

on canola is necessary

(See D290386, 4/22/2005). A summary

of the residue data is presented in Table 8 . The combined residues of flonicamid and metabolites TFNA, TFNA - AM, TFNG following three foliar broadcast applications of the 50% SG formulation of flonicamid at 0.261 - 0.272 lb ai/A , residues (per trial averages, calculated as flonicamid equiv alents ) are : <0.2 - 0.33 3 and <0. 18 - 0.287 ppm for flonicamid and metabolite TFNG, respectively ; residues of TFNA and TFNA - AM are below the LOQ (<0.24 ppm). The combined residues of flonicamid and the three metabolites are <086 - 1.10 ppm. **TABLE 8. Sum ma**  **r y of Residue Data from** **Canola Field Trials with Flonicam id.**  **Com modity**  **Analyte Total**  **Rate (lb ai/A)**  **PHI**

**(days) Residue Levels (ppm**  **flonicam id equivalents)**  **1 ,2**  **n Sam** **ple Min.**  **Sam ple**  **Max. LAFT**  **2 HAFT**  **2 Media**  **n Mean**  **Std.**

**Dev.** Canola seed Flonicamid 0.261 - 0. 272 6 - 8 8 < 0. 2 0. 333 < 0. 2 0.333 0. 2 0. 215 0. 048

TFNA <0.2 4 <0.24 <0.2 4 <0.24 0.24 0.24 0 TFNA - AM <0.2 4 <0.24 <0.2 4 < 0. 24 0.24 0.24 0 TFNG <0. 18 0. 287 <0. 18 0. 287 0.18 0. 195 0.039 Combined 3 <0. 86 1.10 <0. 86 1.1 0. 86 0. 650 0. 245 1 The LOQ was 0.2 ppm for all analytes. V alues reflect per trial averages; n = no . of field trials . Data reflect conversion of quantifiable residues of TFNA, TFNA - AM, and TFNG to parent equivalents by the study reviewer. 2 LAFT = lowest average field trial; HAFT = highest average field trial. 3 Combined residues of flonicamid, TFNA, TFNA - AM, and TFNG calculated using molecular weight conversion factors of 1. 20, 1.21, and 0.92, respectively. Conclusion . The submitted canola field trial data are acceptable . The residues of flonicamid, TFNA, TFNA - AM and TFNG i n/on canola seed harvested at a 6 - to 8 - day PHIfollowing three foliar broadcast applications of the 50% SG formulation of flonicamid at 0.261 - 0.272 lb ai/A were <0.2 - 0.33 3 ppm and <0.2 - 0. 287 ppm for flonicamid and TFNG, respectively . The residues were <LOQ (<0.2 ppm) for TFNA and TFNA - AM in all trials. The combined residues of flonicamid and the three metabolites are <086 - 1.10 ppm. **Processed Food and Feed . 860.1520**  **C anola**  DER Reference: 48657103.de.2 A processing study

was carried out to determine the magnitude of flonicamid , TFNA, TFNA - AM and TFNG residues in canola seed (RAC) and processed canola commodities. In one field trial , Beleaf 50SG was applied as three foliar broadcast applications in/on can ola at an exaggerated rate ( ~3x ) of 0.272 - 0.276 lb ai/A/application for a total rate of 0.821 lb ai/A. Applications were made at 6 - day

RTI s using ground equipment in spray volumes of 15 - 20 gal/A. No adjuvants were added to the spray mixture .Flonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 19 of 28 Canola seed was harvested at an 8 - day PHIan d stored frozen within 29 minut es of collection and were shipped frozen within 28 days of harvest via ACDS truck to the processing fa cility . Processing was completed within 195 days of harvest, and the samples were pl aced in frozen storage (~ - 18 °C) for up to 6 days prior to ship ment via overnight air express to the analy tical laboratory , the Food and Environmental Quality L aboratory

at Washington State University (FEQL; Richland, WA) for analysis. At the analy tical l aboratory , samples were stored frozen (< - 15 °C) until analysis. The processing procedure s simulated commercial operations to generate the required fraction s of canola seed (RAC) into meal and oil . Samples were analy

zed for residues of flonicamid and met abolites TFNA, TFNA - AM, and TFNG using the LC /MS/MS method FMC No. P - 3561M as described under analy tical methods. A number of minor modifications to the method were specified, including changes in clean - up procedure s, reagents, and sample sizes. C onversi on to parent equivalents was not necessary because residues of the metabolites in canola meal and oil were below the LOQ in/on all samples. Briefly , samples of seed were extracted twice with acetonitrile (ACN):water (1:1, v:v), then centrifuged and filt ered. The combined extract was acidified with concentrated HCl and cleaned up using C18 solid phase extraction (SPE), then evaporated to remove ACN. Th e sample was partitioned with ethyl acetate four times ; and the ethyl acetate fractions were combined, reduced by evaporation, and applied to a Carbograph SPE cartridge. The resulting eluate was evaporated to dry ness and re - suspended in 1% formic acid for LC/MS/MS analysis. Samples of meal were extracted with ACN/water as above. The combined aqueous extract was adjusted to volume with water and evaporated to remove ACN, then partitioned with hexane and evaporated to remove hexane. The resulting extract was acidified with concentrated HCl and subjected to partitioning with ethyl acetate followed by Carbo graph SPE cleanup as above. The resulting eluate was evaporated to dry ness and re - suspended in 1% formic acid for LC/MS/MS analysis. Samples of oil were extracted with ACN/water, partitioned with hexane, and acidified as for meal, then subjected to C18 SPE clean - up as for seed. The eluate was partitioned with ethyl acetate four times, and the ethyl acetate fractions were combined, reduced by evaporation and adjusted to volume with 1% formic acid for L C/MS/MS analysis. The LOQ (determined as the LLMV) w as 0.02 ppm for each analy te. The L OD s were c alculated as 1/3 the LOQs . Residue data from the canola processing study are reported in Table 9 . Residues of flonicamid were 0.232 ppm in/on canola seed (RAC) and below the L OQ (<0.02 ppm) in meal and oil. Residues of TFNA, TFNA - AM, and TFNG were each below the LOQ (<0.02 ppm) in/on canola seed, meal, and oil. Combined residues of flonicamid, TFNA, TFNA - AM, and TFNG were <0.292 ppm in/on seed and <0.08 ppm in meal and oil. The processing data indicate tha t combined residues of flonicamid, TFNA, TFNA - AM, and TFNG do not concentrate in meal or oil (processing factor <0.27x).Flonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 20 of 28 The processing factors calculated in this study were less than the maximum theoretical concentration factors for canola of 1.9x for me al and 3.0x for oil (based on separation into components; OCSPP 860.1520, Table 3). **TABLE 9.**  **Residue Data from Canola Processing Study with Flonicam** **id. RAC**  **Processed Com**  **modity Total** 

**Rate (lb ai/A)**  **PHI Residues (ppm** **) 1**  **[Average] Processing Factor**  **2**

**Flo nic**  **** **amid TFNA**  **TFNA**  

** AM** **TFNG Com** ****

**bined 3**  **Flonic**  

** amid** **TFNA TFNA**  ****

**AM TFNG**  **Com******

**bined 3** 

Canola Seed

(RAC) 0.821 8 -- 4 , 0.232 [0.232] <0.02,

<0.02 [<0.02] <0.02,

<0.02 [<0.02] <0.02,

<0.02 [<0.02] <0.292 [<0.292] NA 5

- NA -- -- --

Meal <0.02, <0.02 [<0.02] <0.0 2,

<0.02 [<0.02] <0.02,

<0.02 [<0.02] <0.02,

<0.02 [<0.02] <0.08,

<0.08 [<0.08] <0.09x NC 5 NC NC <0.27x Oil <0.02 <0.02 <0.02 <0.02 <0.08 <0.09x NC NC NC <0.27x 1 The LOQ was 0.02 ppm for all analytes. Averages and combined residues were calculated b y the study reviewer using the LOQ for values reported as <LOQ. The second value for seed and meal reflects the results of redilution (seed) or reinjection (me al). Residues of the metabolites were <LOQ in/on all samples and therefore were not converted to parent equivalents. 2 Processing Factor = [Measured residue for analyte in the processed fraction] / [Measured residue for analyte in the RAC]. 3 Combined residues of flonicamid, TFNA, TFNA - AM, and TFNG . 4 The first value obtained for seed (0.143 ppm) w as rejected by the study director because it was outside the linearity range. 5 NC = Not calculated; residues were below the LOQ (<0.02 ppm for all in analytes) in the RAC and processed fraction ; NA= not available Conclusions . The processing study is acc eptable to satisfy

data requirements. Adequate processing studies on canola are available. The observed processing factors for canola meal and canola oil were each <0.27x. The refore, tolerance s for residues o n meal and oil are not needed. **Submittal of Analytical Reference Standards (860.1650)**  As of April 26, 2012, the analy tical reference standards for flonicamid and the metabolites TFNA, TFNA - AM and TFNG including TFNA - OH and TFNG - AM are available at the EPA National Pesticide Standards Repository wi th expiration dates ranging from 2014

– 2016 (personal communicatio n, D allas Wright and Theresa Cole, ACB, 05/26/2012 ) . **Confined Accumulation in Rotational Crops (**  **860.1850 )**  No new study

was conducted under this guideline and none is required. **Field Acc umulation in Rotational Crops**  **( 860.1900**  **)** No new data was submitted for this guideline and none is required in support of the current petition . **Proposed Tolerances (**  **860.1550 )**  The IR - 4 has proposed the establishment of permanent tolerances for berry low growing subgroup 13 - 07G, cucumber for greenhouse use, and rapeseed, subgroup 20A.Flonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 21 of 28 According to HED’s Interim Guidance on Tolerance Expressions (5/27/09, S. Knizer), the tolerance expression should be stated as follows: Tolerances are established for the residues of the insecticide flonicamid , including its metabolites and degradates, in or on the commodities in the table below. Compliance with the tolerance levels specified below is to be determined by measuring only

the sum of flonicamid [N

- (cyanomethyl) - 4 - ( trifluoromethyl ) - 3 - py ridinecarboxamide ] and its metabolites TFNA (4 - trifluoromethylnicotinic acid), TFNA - AM (4 - trifluoromethylnicotinamide), and TFNG [N - (4 - trifluoromethylnicotinoyl)glycine], calculated as the stoichiometric equivalent of flonicamid , i n or on the following commodities. The submitted magnitude of the residue data for the RACs of the representative crops (strawberry , cucumber, and canola) are adequate to support the tolerance and registration requests for berry , low growing , subgroup1 3 - 07G , cucumber for greenhouse use , and rapeseed subgroup 20A . The OECD spreadsheet calculat ion procedure was used to determine appropriate tolerance levels; see Appendix II. HED recommends for establishment of tolerances using the same tolerance express ion and at the tolerance levels listed in Table 10 below. The petitioner should submit a revised section F reflecting the tolerances and commodity definitions as recommended. **Table 10. Tolerance Sum ma**  **ry for Flonicam id**  **Com mo**  **dity Established/Proposed**  **To lerance**  **(ppm )**  **Recom me**  **nded**

**Tolerance (ppm** **) Com**  **me nts (correct** 

**com mo**  **dity definition)** Berry, low

growing, subgroup 13 - 07G 1.4 1 . 5 1 Cucumber for greenhouse use only 1.3 1.5 2 Vegetable, cucurbit, group 9 2 Rapeseed subgroup 20A 1.5 1.5 3 1 The representativ e commodity for the berry, low growing, subgroup 13 - 07G is strawberry. The OECD spreadsheet calculation procedure gave values of 1.5 ppm for strawberry. 2 A tolerance wa s currently established on cucumber at 0.4 ppm , as a member of the cucurbit vegetable group . The current petition is to increase the tolerance to 1.3 ppm for cucumber grow n in greenhouse only. The OECD spreadsheet calculation procedure gave values of 1.5 ppm for cucumber grown in the greenhouse treated at the proposed label rate by foliar spray. The OECD spreadsheet calculation procedure gave a value of 0.7 ppm for cucumber treated by chemigation in the greenhouse . This tolerance value and the existing tolerance of 0.40 ppm in 40 CFR §180.613 will be covered under the foliar spray treatme nt in greenhouse . 3 The representative commodity for the rapeseed , subgroup 20A is canola. The OECD spreadsheet calculation procedure gave values of 1.5 ppm for canola. No tolerances are required for the processed commoditie s of canola based on the d emonstrated processing factor of <0.27x for each canola meal and canola oil. The maximum theoretical concentration factors for canola meal and canola oil are 1.9x and 3.0x, respectively (OCSPP § 860.1520, Table 3).Flonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 22 of 28 The tolerance expression under § 180. 613(a)(2) for livestock commodities should be stated as: Tolerances are established for the residues of the insecticide flonicamid, including its metabolites and degradates, in or on the commodities in the table below. Compliance with the tolerance l evels specified below is to be determined by measuring only

the sum of flonicamid [N - (cyanomethyl) - 4 - (trifluoromethyl) - 3 - py ridinecarboxamide] and its metabolites TFNA (4 - trifluoromethylnicotinic acid), and TFNA - AM (4 - trifluoromethylnicotinamide), calcul ated as the stoichiometric equivalent of flonicamid, in or on the following commodities. The existing livestock commodity tolerances are adequate. There are currently

no Codex or Canadian maximum residue limits (MRL s) established for residues of flonicamid in crop or livestock commodities. An International Residue L imit Status sheet (IRL) is attached to this Summary Document (APPENDIX I) . Attachments: Appendix I - International Residue L imit Status sheet Appendix II - Tolerance Assessment Calculations Template Version September 2005Flonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 23 of 28 **Appendix I International Residue Limits**  

### Flonicamid (PC Code 128016; 04/26/2012 ) Summary of US and International Tolerances and Maximum Residue Limits Residue Definition : US Canada Mexico 2 Co dex 3 40 CFR 180.613: Plant : flonicamid [N - (cyanomethyl) - 4 - (trifluoromethyl) - 3 -py

ridinecarboxamide] and its metabolites TFNA [4 - trifluoromethylnicotinic acid], TFNA - AM [4 - trifluoromethylnicotinamide] , and TFNG [N - (4 - triflu oromethylnicotinoyl)glycine] Livestock: residues of flonicamid [N - (cyanomethyl) - 4 - (trifluoromethyl) - 3 -py

ridinecarboxamide], and its metabolites TFNA [4 - trifluoromethylnicotinic acid] and TFNA - AM [4 - trifluoromethylnicotinamide] None None

Commodity 1 Tolerance (ppm) /Maximum Residue Limit (mg/kg) US Canada Mexico 2 Codex 3 Berry , low growing, subgroup 13 - 07G 1.5 Vegetable, cucurbit, group 9 1.5 Rapeseed Subgroup 20A 1.5

Completed: M. Negussie; 05/01/2012 1 Includes only commodities of interest for this action. Tolerance values should be the HED recommendations and not those proposed by the applicant. 2 Mexico adopts US tolerances and/or Codex MRLs for its export purposes. 3 * = absent at the limit of quantitation; Po = postharv est treatment, such as treatment of stored grains. PoP = processed postharvest treated commodity, such as processing of treated stored wheat. (fat) = to be measured on the fat portion of the sample. MRLs indicated as proposed have not been finalized by th e CCPR and the CAC. 1 Includes only commodities of interest for this action. Tolerance values should be the HED recommendations and not those proposed by the applicant.Flonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 24 of 28 

### A **ppendix II Tolerance Assessment Calculations**  For each of the crops listed belo w, the OECD calculator was used for calculating recommended tolerances. As specified in the OECD document , the average residue value was used The rounding procedures specified in the OECD guideline were also used. For each of the crops listed below , the field trials reflect the proposed application rate s and samples were collected at the proposed pre - harvest intervals. **Berry, L ow**  **G rowing,**  **S ubgroup 13**  **- 07G**  The dataset used to establish a tolerance for residues of flonicamid in/on berry , low growing con sisted of field trial data representing total application rate of 0.263 - 0.280 lb ai/A ( 3 applications at 0.086 - 0.094 lb ai/A/application) with a 0 - day PHI . The representative c rop of the low growing berry

is strawberry . T he average residue values for strawberry crop field trial used to calculate the tolerance s are provided in Table II - 1 and these values were entered in the OECD calculator . Using the OECD calculator, the recommended tolerance is 1.5 ppm . A crop group tolerance is appropriate for berry lo w growing subgroup 13 - 07G . The re commended tolerance is slightly higher than the proposed ( 1.4 ppm). **Cucumber ( G**  **reenhouse)** The dataset used to establish a tolerance for residues of flonicamid in/on greenhouse grown cucumber consisted of greenhouse trial data representing two methods of application : (a) foliar application rates of 0. 262 - 0.29 1 lb ai/A ( 2 foliar applications at 0.129 - 0.147 lb ai/A/application) with a 6 - 7 - days RTIand 0 - days PHI) and (b) application by simulated chemigation to the rock wool substrate in which the cucumber plants were grown using sy ringe) at rates of 0.264 - 0.269 lb ai/A (2 chemigation application at 0.130 - 0.134 lb ai/A/application) with a 6 - to 7 - day RTIand 0 - days PHI . The average residue values for cucumber greenhouse trial (a) and (b) used to calculate the tolerances are provided in Table II - 1 and these values were entered in the OECD calculator. Using the OECD calculator, the recommended tolerance is 1.5 ppm. The recommended tolerance for cucurbit vegetables, group 9, is higher than the proposed (1. 3 ppm) for greenhouse cucumbers . The existing tolerance for cucurbit vegetables is 0.4 ppm. This is based on the evaluation of crop field trial data for summer squash, cantaloupe, and cucumber (D290386, A. Acierto, 04 /22/2005). The highest residues were 0.17 ppm on squash, 0.34 ppm on cucumber, and 0.25 ppm on cantaloupe. The recommended tolerance of 1.5 ppm for cucurbit vegetables is appropriate for the representative commodities.Flonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 25 of 28 **Rapeseed, Subgroup 20A** The dataset used to establish a tolerance for residues of flonicamid in/on rapeseed consisted of field trial data representing total application rate of 0.261 - 0.272 lb ai/A (3 applications at 0.085 - 0.092 lb ai/A/application) with 6 - to 8 - day RTIand 6 - to 8 - day

and 6 - to 8 - day PHI . The representative crop is canola . The average residue values for the canola field trial used to calculate the tolerances are provided in Table II - 1 and these values were entered in the OECD calculator. Using the OECD calculator, the rec ommended tolerance is 1.5 ppm. A crop group tolerance is appropriate for rapeseed subgroup 20A. The proposed tol erance of 1.5 ppm is appropriate. **Flonicamid Strawberry**  **USA 0.258**  **- 0.282 lb ai/A**  **Total number of data (n)** 7 **Percentage of censored d ata**  0% **Number of non -**  **censored data** 7 **Lowest residue** 0.200 **Highest residue** 0.710 **Median residue** 0.410 **Mean** 0.446 **Standard deviation (SD)** 0.193 **Correction factor for censoring (CF)** 1.000 **Proposed MRL estimate**

**- Highest residue**  0.710

**- M** **ean + 4 SD** 1.219

**- CF x 3 Mean**  1.337 **Unrounded MRL** 1.337 **Rounded MRL 1.5**  High uncertainty of MRL estimate. [Small dataset] **Residues (mg/kg) n**  **0.2 1**  **0.25 1**  **0.36 1**  **0.41 1**  **0.56 1**  **0.63 1**  **0.71 1** Flonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 26 of 28 **Flonicamid Cucumber**  **(Member o f Cucurbit Crop Group)** 

**USA/Canada Foliar,0.262**  **- 0.291lb ai/A**  **, 0 -**  **day PHI Total number of data (n)**  4 **Percentage of censored data** 0% **Number of non -**  **censored data** 4 **Lowest residue** 0.114 **Highest residue** 0.619 **Median residue** 0.164 **Mean** 0.265 **Standar d deviation (SD)**  0.240 **Correction factor for censoring (CF)** 1.000 **Proposed MRL estimate**

**- Highest residue**  0.619

**- Mean + 4 SD**  1.224

**- CF x 3 Mean**  0.795 **Unrounded MRL** 1.224 **Rounded MRL 1.5**  High uncertainty of MRL estimate. [S mall dataset] **Residues (mg/kg) n**  0.114 1 0.121 1 0.206 1 0.619 1Flonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 27 of 28 **Flonicamid Cucumber**  **(Member of Cucurbit Crop Group)**

**USA and Canada Chemigation 0.264**  **- 0.269 lb ai/A (0.296**  **- 0.302 kg/ha, 0**  **- day**  **PHI Total number of data (n)**  4 **Percentage of censored data** 0% **Number of non -**  **censored data** 4 **Lowest residue** 0.079 **Highest residue** 0.341 **Median residue** 0.175 **Mean** 0.192 **Standard deviation (SD)** 0.110 **Correction factor for censoring (CF)** 1.000 **Proposed MRL estimate**

**- Highest residue**  0.341

**- Mean + 4 SD**  0.633

**- CF x 3 Mean**  0.577 **Unrounded MRL** 0.633 **Rounded MRL 0.7**  High uncertainty of MRL estimate. [Small dataset] **Residues (mg/kg) n**  0.079 1 0.154 1 0.195 1 0.341 1Flonicamid Summary of Analytical Chemistry and Residue Data DP# D396902

Page 28 of 28 **Flonicamid Canola**  **Region / USA**  **0.261 -**  **0.272 lb ai/A PHI = 6 -**  **8 days Total number of data (n)**  8 **Percentage of censored data** 75% **Number of non -**  **censored data** 2 **Lowest residue** 0.860 **Highest residue** 1.100 **Median residue** 0.860 **Mean** 0.895 **Standard deviation (SD)** 0.08 4 **Correction factor for censoring (CF)** 0.500 **Proposed MRL estimate**

**- Highest residue**  1.100

**- Mean + 4 SD**  1.231

**- CF x 3 Mean**  1.343 **Unrounded MRL** 1.343 **Rounded MRL 1.5**  High uncertainty of MRL estimate. [High level of censorin g] **Residues (mg/kg) n**  < 0.86 6 0.9 1 1.1 1