Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 1 of 45 **UNITED STATES ENVIRONMENTAL PROTECTION AGENCY**

**WASHINGTON, DC 20460 OFFICE OF CHEMICAL S**  **AFETY AND POLLUTION PREVENTION**  **MEMORANDUM DATE**  **: 16 June 2013**  **SUBJECT: Methoxyfenozide.**  Petition to Establish Permanent Tolerances (Associated with

Section 3 Registration) for Residues Resulting from Food/Feed Uses of the Insecticide on Herbs (Subgroup 19A) Except Chives , Caneberries (Subgroup 13 - 07A) , Dates and Sorghum ; to Update the Pome Fruits and Fruiting Vegetables Crop Group s ; to Extend the Tolerance s in Grapes and Strawberries to Th eir Respective Subgroups, and in Avocadoes to Various Tropical Tree Fruits ; to Remove the Tolerance s in Dried Shelled Peas and Beans , and Add a Tolerance in Subgroup 6C ; and to Establish Rotational Crop Tolerances in Chives, Spices (Subgroup 19B ) , and the Rapeseed (20A) and Sunflower (20B) Oilseed Subgroups . Summary

of Analy tical Chemistry

and Residue Data. **PC Code:** 121027 **DP Barcode**  **:** D407 75 8 **Decision N umber**  **:** 4 721 4 2 **Registration Number**  **:** 62719 - 44 2 **P etition**  **:** 2 E 8 118 **Regulatory Action:** Section 3 **Risk Assessment Type:** NA **Case Number**  **:** 74 3 1 **T XR**  **Number :**  NA **CAS Number**  **:** 161050 - 58 - 4 **MRID Numbers**  **:** 48994101 - 04 **40 CFR:** § 180. 54 4 **FROM:** William T. Drew, Chemist

Risk Assessment Branch II (RAB2) Health Effects Division ( HED), 7509P **THROUGH:** Elizabeth Holman , Physical Scientist

RAB2/HED , 7509P **TO:** Barbara Madden and Laura Nollen , RM Team 5

Risk Integration, Minor Use, and Emergency Response Branch (RIMUERB) Registration Division (RD), 7505PMethoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 2 of 45 **Table of Contents** 1.0 Executive Summary ................................ ................................ ................................ .............. 4 2.0 Regulatory

Recommendations ................................ ................................ .............................. 7 2.1 Data Deficiencies/Data Needs ................................ ................................ .......................... 8 2.2 Tolerance Considerations ................................ ................................ ................................ .. 8 2.2.1 Enforcement Analy tical Method/Multiresidue Methods ................................ .......... 8 2.2.2 Recommended Toleran ces ................................ ................................ ........................ 8 2.2.3 Revisions to Petitioned - For Tolerances ................................ ................................ .... 9 2.2.4 International Harmonization ................................ ................................ ................... 10 2.3 L abel Recommendations ................................ ................................ ................................ 11 2.4 Submittal of Analy tical Reference Standards (860.1650) ................................ ............. 11 3.0 Chemical Identity ................................ ................................ ................................ ............... 12 3.1 Nomenclature ................................ ................................ ................................ ................. 12 3.2 Phy sic o chemical Characteristics ................................ ................................ .................... 13 3.3 Pesticide Use Pattern/Directions for Use (860.1200) ................................ .................... 13 4.0 Metabolite/Degradate Residue Profile ................................ ................................ ............... 14 4.1 Nature of the Residue ................................ ................................ ................................ ..... 14 4.1.1 Summary

of Plant and

/or Livestock Metabolism (860.1300) ................................ . 15 4.1.2 Summary

of Confined Rotational Crops (860.l850) ................................ ............... 16 4.1.3 Summary

of Rat Metabolism ................................ ................................ .................. 16 4.1.4 Summary

of Environmental Degradation ................................ ............................... 17 5.0 Residue Profile ................................ ................................ ................................ ................... 17 5.1 Residue Anal ytical Methods (860.1340) ................................ ................................ ...... 17 5.1.1 Data Collection Methods ................................ ................................ ........................ 17 5.1.2 Multi - Residue Methods (860.1360) ................................ ................................ ........ 22 5.1.3 Tolerance Enforcement Methods ................................ ................................ ............ 22 5.2 Storage Stability

(860.1380) ................................ ................................ .......................... 23 5.3 Residue Data ................................ ................................ ................................ .................. 26 5.3.1 Crop Field Trials (860.1500) ................................ ................................ .................. 26 5.3.2 Field Rotational Crops (860.1900) ................................ ................................ ......... 30 5.3.3 Processed Food and Feed (860.1520) ................................ ................................ ..... 30Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 3 of 45 5.3.4 Meat, Milk, Poultry and Eggs (860.1480) ................................ .............................. 32 5.3.5. Food Handling (86 0.1460) ................................ ................................ ...................... 33 5.3.6 Water, Fish and Irrigated Crops (860.1400) ................................ ........................... 33 5.4 Food Residue Profile ................................ ................................ ................................ ...... 33 6.0 Tolerance Derivation ................................ ................................ ................................ ......... 33 Attachment 1: International Resi due Limit Status sheet ................................................37 Attachment 2: OECD MRL(Tolerance) Assessment Calculations ...................................39Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 4 of 45 **1.0 Executive Summary**  Methox yf enozide (with CAS name 3 - methoxy- 2 - methylbenzoic acid 2 - (3,5 - dimethylbenzoyl) - 2 - (1,1 - dimethylethyl)hydrazide, and CAS number 161050 - 58 - 4) is a diacylhydrazine insecticide used on a wide variety of food and feed crops for the control of lepidopterou s pest species. Permanent tolerances are established for residues of methoxyfenozide in or on a wide variety of plant commodities, at levels ranging from 0.02 ppm in peanuts and tuberous/corm vegetables (subgroup 1D), to 160 ppm in soy bean aspirated grain fractions (40CFR §180.544[a][1]). Permanent tolerances are also established for residues of methox yfenozide in the milk, meat and fat of livestock (40CFR §180.544[a][1]), and for the combined residues of the parent and its glucuronide conjugate (RH - 141,5 18) in eggs and meat by products at 0.02 - 0.40 ppm (40CFR §180.544[a][2]). Additionally , p ermanent tolerances for methoxyfenozide are established in high - moisture rotational crops (40CFR §180.544[ d][1]), and for the combined residues of the parent and its m etabolites RH - 151,055, RH - 152,072 and RH - 117,236 in low - moisture rotational crops (40CFR §180.544[d][2 ]) . Time - limited tolerances (associated with Section 18 emergency exemptions) were established for residues of methoxyfenozide in sorghum forage, grain and stover (40CFR §180.544[b]); these tolerances expire d on 31 December 2012. The Interregional Research Project Number 4 (IR- 4) has submitted a petition requesting the establishment of permanent tolerance s for residues of methoxyfenozide in or on date s ; c aneberries ( subgroup 13 - 07A) ; grain s orghum forage , stover and grain ; sweet s orghum forage , stover , grain and stalk s ; aspirated grain fractions (AGF) , based on sorghum data; dried shelled p ea s and bean s , except soy bean s ( subgroup 6C ) , except blackeyed pea s and southern pea s ; fresh h erb s ( subgroup 19A ) , except chive s ; and dried h erb s ( subgroup 19A) , except chive s . Tolerances were requested in the updated crop groups 8 - 10 and 11 - 10 (from groups 8 and 11, respectivel y) , and in the updated subgroups 13 - 07F and 13 - 07G (from gra p e s and strawberries , respectivel y) . Tolerances in sugar apple s , cherimoya s , atemo ya s , custard apple s , ilama s , soursop s and biriba s we re also requested , based on translation of avocado residues. Additionally , rotational crop tolerances in the rapeseed subgroup ( 20A ) and the s unflower subgroup ( 20B ) were requested . The proposed new uses in dates, caneberries, sorghum and herbs are supported b y m agnitude - of - residue data generated by IR- 4. Other changes are supported by

data pr eviously

reviewed b y the Agency in 2009. The requested rotational crop tolerances in the rapeseed and sunflower sub group s are based on 2012 recommendations by EPA. The petition propose s the removal of the ( expired) temporary tolerances in grain sorghum commodities , and their replacement with permanent tolerances in sweet and grain sorghum commodities . The tolerance in AGF would be increased from 2.0 to 120 ppm. The tolerance of 0.5 ppm in dried shelled peas and beans, except soy bean s (subgroup 6C) was proposed at the Agency's request to better harmonize with existing Codex MRL s. The existing tolerances in dried beans and dried peas would be remove d concurrentl y with the establishment of tolerance in subgroup 6C . The tolerance in okra would be remove d concurrentl y with the update of crop group 8 to crop group 8 - 10. The tolerance s in grapes and strawberries would be remove d concurrently

with the establishment of the tolerance s in crop subgroups 13 - 07F and 13 - 07G , respectivel y. The primary crop tolerance in coriander leaves , along with the rotational cropMethoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 5 of 45 tolerance in h erb s and spices ( group 19 ) , except coriander leaves , would be remove d concurrently

with the establishment of the primary crop tolerance in subgroup 19A , except chives . Although not prop osed in the petition, rotational crop tolerances would necessaril y be established in chives and in spices (subgroup 19B) upon establishment of the primary crop tolerance in subgroup 19A, except chives. This summary document addresses the data supporting the proposed tolerances for residues of methoxyfenozide in the various commodities listed above. Crop Field Trials : To support the requested new use s , field trials were conducted on basil, caneberries, dates and sorghum . Five basil field trials were conducted in the US and Canada during the 2009 growing season in North American Free Trade Agreement (NAFTA) Growing Zones 2 (NC), 3 (FL), 5A (WI), 9 (NM) and 12 (BC). Following 4 foliar directed or broadcast applications of the f lowable concentrate (FlC) formulation containing 2 pounds of active ingredient per gallon (lb ai/gal) to basil at total rates of 0.988 - 1.032 lb ai per acre (lb ai/A), residues (and per- trial averages) of methoxyfenozide were 9.26 - 47.2 (9.88 - 43.4) ppm in fresh basil, and 56.3 - 194 (60.5 - 188) ppm in dried basil harvested at a 1 - day pre - harvest interval ( PHI) . These field trial data support a tolerance of 8 0 ppm in fresh herbs ( subgroup 19A) except chives , and a tolerance of 40 0 ppm in dried herbs (subgroup 19 A) except chives . However, HED has determined that it would be preferable to set a tolerance in the entire crop sub group (herbs subgroup 19A , except chive s) at 400 ppm. Six caneberry

field trials were conducted in the US during the 2010 growing season in NAFTA Growing Zones 2 (NC, blackberry), 5A (M I, blackberry), 10 (CA, blackberry) and 12 (OR, one trial on blackberry , and two trials on raspberry). Following 3 foliar directed applications of the 2 lb ai/gal FlC formulation to caneberries at total rates of 0.744 - 0.778 lb ai/A, residues (and pertrial averages) of methoxyfenozide were 0.62 - 2.5 (0.68 - 2.5) ppm in berries that were harvested at a 3 - day PHI. These field trial data support a tolerance of 6 .0 ppm in caneberries (subgroup 13 - 07A) . Three date field trials were conducted in the US during the 2010 growing season in NAFTA Growing Zone 10 (CA). Following 3 foliar directed applications of the 2 lb ai/gal FlC formulation at total rates of 0.501 - 0.933 lb ai/A, residues (and per - trial averages) of methoxyfenozide were 1.5 - 3.3 (1.6 - 3.1) ppm in dry fruit harvested at a 7 - day PHI . These field trial data support a tolerance of 8.0 ppm in dates. Twelve grain sorghum field trials were conducted in the US during the 2009 growing season in NAFTA Growing Zones 2 (NC), 4 (AR), 5 (ND 3 trials; SD 1 trial), 6 (TX, 2 trials), 7 (NE), 8 (TX) and 10 (NM, 2 trials). There was also 1 sweet sorghum field trial c onducted in Growing Zone 6 (TX) during the same growing season. Following 4 foliar broadcast or directed applications of the 2 lb ai/gal FlC formulation to grain sorghum at total rates of 0.478 - 0.494 lb ai/A, residues (and per - trial averages) of methoxyfenozide were 0.70 - 5.6 (0.77 - 5.0) ppm inMethoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 6 of 4 5 sorghum forage harvested at a PHI of 2 - 4 days, 0.1 5 - 2.6 (0.15 - 2.3) ppm in sorghum grain harvested at a PHI of 11 - 23 day s, and 0.29 - 9.7 (0.45 - 7.6) ppm in sorghum stover harvested at a PHIof 21 - 23 day s. Following 4 foliar broadcast applications of the 2 lb ai/gal FlC formulation to sweet sorghum (onl y 1 trial) at a total rate of 0.481 lb ai/A, residues (and per- trial average) of methoxyfenozide were 0.045 - 0.18 (0.11) ppm in sorghum stalks harvested at a PHI of 3 day s. These field trial data support tolerance s of 6 .0 ppm in both sweet and grain sorghum grain , tolerance s of 15 ppm in both sweet and grain sorghum forage (as well as sweet sorghum stalks), and tolerances of 20 ppm in both sweet and grain sorghum stover . Processing Studies : Because there are no processed commodities for caneberries or dates, processing studies were not required for these raw agricultural commodities (RACs). The processed commodity

for basil is dried basil, samples of which were produced at the field trial sites, and subsequently

analyzed along with the fresh basil samples. P rocessing data were submitted for sorghum (sweet sorghum s yrup and AGF) . Residues of methoxyfenozide were 1.1 and 0.48 ppm in sorghum stalks and grain (RACs) harvested at PHIs of 3 and 21 day s, respectively , following the last of 4 foliar broadcast applications of the 2 lb ai/gal FlC formulation of methoxyfenozide at a total rate of 0.481 lb ai/A. Residues of methoxyfenozide were 1.1 and 17 ppm in sorghum sy rup and sorghum AGF, re spectivel y. These data indicate that methoxyfenozide did not concentrate in sweet sorghum s yrup (1 X processing factor) , but did concentrate in sorghum AGF (35 X processing factor) . Ergo, a tolerance in sweet sorghum sy rup is not required; the processing data support a tolerance of 120 ppm in AGF. Residue Analytical Methods : Validated methods are available for the enforcement of methoxyfenozide tolerances. Adequate method s w ere used for the quantitation of methoxyfenozide residue s in samples from the various crop field trial and processing studie s, based on acceptable method validation and concurrent recovery data. Storage Stability : Adequate storage stability data are available to support the storage durations and conditions of samples from the submitted field trial and processing studies . Meat, Milk, Poultry and Eggs: The current action for the proposed use s will not result in revisions to the existing tolerances in livestock commodities . MRL Harmonization : Codex has not established maximum residue limits (MRL s) in any of the proposed new uses . As such, there are no harmonization issues associated with Codex for the proposed new uses in the current action. Canada’s Pest Management Regulatory Agency (PMRA) has established MRL s in fresh Chinese chive leaves and fresh chive leaves at 5 mg/kg. There are no Canadian MRL s in dates, caneberries or sorghum commodities. However, PMRA and the Agency

are jointly

reviewing the basil and caneberry data in the current action ; EPA and PMRA will attempt to harmonize the re commended tolerances/MRLs in herbs and caneberries .Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 7 of 45 Codex has established MRL s in grapes at 1 mg/kg , in strawberries and pome fruits at 2 mg/kg , in avocado es at 0.7 mg/kg , and in papaya s at 1 mg/kg . The recommended tolerance of 2 .0 ppm in the updated pome fruits group ( 1 1 - 1 0), increa s ed from the current tolerance of 1.5 ppm in group 11 , would be harmonized with the Codex MRL . The recommended tolerance of 1.0 ppm in small vine - climbing fruit, except fuzzy kiwifruit ( subgroup 13 - 07F ), translated from grape data, would be harmonize d with the Codex MRL in grapes . The recommended tolerance of 2.0 ppm in low - growing b erries ( subgroup 13 - 07G), translated from strawberry data , and increased from the current tolerance of 1.5 ppm in strawberries , would be harmonized with the Codex MRLin strawberries. The recommended tolerance of 0. 6 0 ppm in various tropical tree fruits , translated from avocado data (there is also a tolerance of 0.6 ppm in papaya) , would not be harmonized with the Codex MRL s in avocadoes or papayas. The recommended tolerance of 0.5 0 ppm in dried shelled pea s and bean s, except soy bean s (subgroup 6C) wa s proposed at the Agency's request to better harmonize with the existing Codex MRLof 0.5 mg/kg in dried beans . This tolerance would replace the current tolerance s of 0.24 ppm in dried beans, and 2.5 ppm in dried peas , which would both be remove d . **2.0 Regulatory Recom**  **m endations**  HED has examined the residue chemistry database for methoxyfenozide . Pending submission of a revised Section F (to propose tolerance levels and additional commodities in accord ance with those recommended b y HED , and to correct th e commodity definition for the h erb subgroup 19A) , there are no residue chemistry issues that would preclude establishing tolerance s in the requested commodities . The recommended tolerance s are listed in Ta ble 2.2.2 , below . **Note to RD:** Analy

tical standard s f

or methoxyfenozide and its 4 metabolites are currently available at EPA’s National Pesticide Standards Repository (NPSR) . However, the RH - 152072 metabolite standard expired on 10 October 2010, and the RH - 141518 metabolite standard expired on 26 July

2013 ; neither ha s been replenished by the registrant. Additionally, the RH 117236 metabolite standard expires on 3 September 2013 . The registrant should resubmit new anal ytical reference standard s , or updated certificate s of anal ys is (COA s ) , for all 3 of the se standard s , most urgently

for the expired RH - 152072 and RH - 141518 , but also for RH - 117236 before its expiration date. S ee Section 2.4, below . **Note to RD:** Concurrent with the establishment of permanent tolerances in sweet and grain sorghum commodities (40CFR §180.544 [a] [1] ), the paragraph referring to, and the table containing, the time - limited tolerances in grain sorghum commodities (40CFR §180. 544 [b]) should be removed, and replaced with “[Reserved]”. Concurrent with the establishment of the tolerance in subgroup 6C (except blackeyed and southern peas) , the tolerances in dried beans and dried peas should be removed (40CFR §180.544[a] [1] ).Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 8 of 45 Concurrent w ith the establishment of the tolerance in group 8 - 10, the tolerance s in okra and group 8 should be removed (40CFR §180. 544 [a] [1] ). Concurrent with the establishment of the tolerance in group 11 - 10, the tolerance in group 11 should be removed (40CFR §180.544[a][1]). Concurrent with the establishment of the tolerance in subgroup 13 - 07F, the tolerance in grapes should be removed (40CFR §180. 544 [a] [1] ). Concurrent with the establishment of th e tolerance in subgroup 13 - 07G , the tolerance in strawberri es should be removed (40CFR §180.544[a] [1] ). Concurrent with the establishment of the tolerance in subgroup 1 9A (except chives) , the tolerance in coriander le av es should be removed (40CFR §180.544[a] [1] ) , and tolerances in subgroup 19B and chives should be established (40CFR §180.544[ d][ 2 ]) . **2.1 Data Deficiencies/Data Needs**  None. **2.2 Tolerance Con**  **sid erations**  **2.2.1 Enforcement Analytical Method** **/Multiresidue Methods** Adequate methods using high performance liquid chromatography with ultraviolet or mass spectrometric detection (HPL C/UV or /MS) are available for enforcing the current tolerances for methoxyfenozide in primary and rotational crops, and in animal commodities. Depending on the pl ant commodity , the limits of quantitation (L OQs) for methox yf enozide in primary

crop commodities are 0.01 - 0.05 ppm. Data concerning the recovery of methox yf

enozide using the FDA multiresidue method protocols ( PAM Volume I

) were previously

submitted to, and reviewed b y, HED. Methoxyfenozide was not recoverable b y any of these procedures. The data were forwarded to FDA for evaluation, and the updating of PAM Volume I . **2.2.2 Recommended Tolerances**  **TABLE 2.2.2**  **Tolerance Summary for Methoxyfenozide**  **. Comm**  **odity as Proposed by the** 

**Petitioner Proposed**  **Tolerance (ppm) Recommended** 

**Tolerance (ppm) Comments;**  **Correct**

**Commodity Definition** Herb subgroup 1 9A, fresh, except chive s 70 400 Herb subgroup 19A, except chive Herb subgroup 19A, dried , except chive s 400 Caneberry subgroup 13 - 07A 6.0 6.0Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 9 of 45 **TABLE 2.2.2**  **Tolerance Summary for Methoxyfenozide**  **. Comm**  **odity as Proposed by the** 

**Petitioner Proposed**  **Tolerance (ppm) Recommended** 

**Tolerance (ppm) Comments;**  **Correct**

**Commodity Definition** Date 7.0 8.0 One date and all sorghum O ECD calculator inputs were increa sed to account for field trials conducted at half (date) or 2⁄3 (sorghum) the proposed use rate (based on OECD’s preliminary guidance on proportionality of sample residues to application rate ). Sorghum, grain, forage 9.0 15 Sorghum, grain, stover 15 20 Sorghum, grain, grain 4.0 6.0 Sorghum, sweet, forage 9.0 15 Sorghum, sweet, stover 15 20 Sorghum, sweet, grain 4.0 6.0 Sorghum, sweet, stalk 9.0 15 Grain, aspirated grain fractions 80 120 Pea and bean, dried shelled, except soy bean, subgroup 6C, except pea, blackeyed, seed and pea, southern, seed 0.5 0.5 0 Revise tolerance from 0.5 ppm to 0.50 ppm . Fruit, small, vine clim

bing, except fuzzy kiwifruit, subgroup 13 - 07F 1.0 1.0 Berry, low

growing, subgroup 13 - 07G, except cranberry 1.5 2.0 Tolerance h armonize d with Codex MRL in strawberry. Fruit, pome, group 11 - 10 1.5 2.0 Tolerance harmonized with Codex MRL in pome fruits. Vegetable, fruiting, group 8 - 10 2.0 2.0 Sugar apple 0.6 0.60 Revise tolerance s from 0.6 ppm to 0. 6 0 ppm . Cherimoya 0.6 0.6 0 Atemoya 0.6 0.6 0 Custard apple 0.6 0.6 0 llama 0.6 0.6 0 Soursop 0.6 0.6 0 Biriba 0.6 0.6 0 Rapeseed subgroup 20A 1.0 1.0 Rotational crop tolerances. Sunflower subgroup 20B 1.0 1.0 Spice subgroup 19B* None 4.5 Chive* None 4.5 * These commodities were not proposed by the petitioner , but are recommended by HED . **2.2.3 Revisions to Petitioned**  **- For**  **Tolerances** In fresh herbs, subgroup 19A ( except chives), the petitioner proposed a tolerance of 70 ppm, based on the Organization of Economic Development and Cooperation’s (OECD’s) tolerance calculation procedure . T he petitioner entered all 10 individual sample residues into the MRL calculator . When the average residues from each of the 5 basil field trials were entered, as the OECD guidance stipulates, the resulting recommended tolerance would be 80 ppm. In dried herbs, subgroup 19A (except chives), the petitioner proposed a tolerance of 40 0 ppm, based on OECD’s tolerance calculation procedure. However, the A gency has determined that setting separate subgroup 19A tolerances in fresh and dried commodities is not f easible from a regulatory

perspective. Therefore, HED recommends setting the tolerance in the entire subgroup 19A (both fresh and dried commodities ) , except chives, at the higher level of 400 ppm.Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 10 of 45 In dates , the petitioner proposed a tolerance of 7 . 0 ppm , based on 4 date field trials and the OECD’ s tolerance calculation procedure. However, HED determined that only 3 of the trials were trul y independent. The 4 sample residues from the 2 trials deemed to be non - independent were averaged together as one input into the MRL calculator. Also, the total application rate at one of the other trials was only half the proposed maximum seasonal use rate , a difference of >25% . Ergo, the residue values from this trial were doubled, per OECD’s preliminary guidance on proportionality

of sample residues to application rate ( decision from the minutes of HED’s Chemistry

Science Advisory

Council meeting of 28 March 2012 ). When the average of these residues , along with the average residues from each of the other 2 field trials were entered into the MRLcalculator , the resulting recommended tolerance wa s 8 . 0 ppm. In sorghum commodities , the petitioner proposed tolerance s of 9.0, 15 and 4.0 ppm in the forage, stover and grain, respectively , of both grain and sweet sorghum, and 9.0 ppm in sweet sorghum stalks, based on OECD’s tolerance calculation procedure . A tolerance of 80 ppm in sorghum AGF was proposed , based on the sorghum processing study . However, the total application rate at the sorghum field trials was only tw o thirds the proposed maximum seasonal use rate, a difference of >25%. Ergo, the residue values from th e trial s were increas ed by half , per OECD’s preliminary

guidance on proportionality (ChemSAC meeting ; 28 March 2012) . When these values were entered into the MRLcalculator , the resulting recommended tolerance s were 15, 20 and 6.0 ppm in the forage, stover and grain, respectively , of both grain and sweet sorghum , and 15 ppm in sweet sorghum stalks. Similarly , when the HAFT from the sorghum field trials (2.25 ppm) wa s increased b y half , and multiplied by

the AGF processing factor (35X), the resulting recommended tolerance was 12 0 ppm in sorghum AGF. Instead of the proposed tolerance s in the various tropical tree fruits (0. 6 ppm), HED recommends establishing the tolerance s at 0. 6 0 ppm, in order to avoid the situation where a field sample containing residues significantly above the tolerance (0. 6 4 ppm, for example) would be considered non - violative. For the same reason , HED recommends that the proposed tolerance of 0. 5 ppm in subgroup 6C (except blackeyed and southern peas ) be revised to 0. 5 0 ppm. **2.2.4 International Harmonization**  Codex has not established MRL s in any of the proposed new uses. As such, there are no harmonization issues associated with Codex for the proposed new uses in the current action. Canada’s PMRA has established MRL s in fresh Chinese chive leaves and fresh c hive leaves at 5 mg/kg. There are no Canadian MRL s in dates, caneberries or sorghum commodities. However, PMRA and the Agency

are jointly

reviewing the basil and caneberry data in the current action; EPA and PMRA will attempt to harmonize the recommended tolerances/MRL s in herbs and caneberries. Codex has established MRL s in grapes at 1 mg/kg, in strawberries and pome fruits at 2 mg/kg, in avocadoes at 0.7 mg/kg, and in papayas at 1 mg/kg. The recommended tolerance of 2.0 ppm inMethoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 11 of 45 the updated pome fruit s group (11 - 10), increased from the current tolerance of 1.5 ppm in group 11, would be harmonized with the Codex MRL . The recommended tolerance of 1.0 ppm in small vine - climbing fruit, except fuzzy kiwifruit (subgroup 13 - 07F), translated from grape data, would be harmonized with the Codex MRLin grapes. The recommended tolerance of 2.0 ppm in low - growing berries (subgroup 13 - 07G), translated from strawberry data, and increased from the current tolerance of 1.5 ppm in strawberries, would be harmonized with the Codex MRLin strawberries. The recommended tolerance of 0.60 ppm in various tropical tree fruits, translated from avocado data (there is also a tolerance of 0.6 ppm in papaya), would not be harmonized with the Codex MRL s in avocadoes or papayas. The recommended tolerance of 0.50 ppm in dried shelled peas and beans, except soy beans (subgroup 6C) was proposed at the Agency's request to better harmonize with the existing Codex MRLof 0.5 mg/kg in dried beans. This tolerance would replace the current to lerances of 0.24 ppm in dried beans, and 2.5 ppm in dried peas, which would both be removed. **2.3 Label Recommendations**  N one. **2.4 Submittal of Analytical Reference Standards**  **( 860.1650**  **)** The anal ytical standard for methoxyfenozide (RH - 112485), with an expiration date of 17 October 2014, is currently available in the EPA’s NPSR, per Email communication from Theresa Cole of the Biological and Economic Anal ys is Division’s (BEAD’s) Anal ytical Chemistry Branch (ACB ) of 9 M ay

201 3 . However, the RH - 152072 metabolite standard expired on 10 October 2010, and the RH - 141518 metabolite standard expired on 26 July 2013; neither has been replenished b y the registrant. Additionally , the RH - 117236 metabolite standard expires on 3 September 2013. The registrant is required to maintain reasonable amount s of the anal ytical reference standard s for methoxyfenozide and its 4 metabolites . N ew reference standard s, or updated COAs, should be sent to the ACB, which is located at Fort Meade, MD. Itshould be sent to the attention of either Theresa Cole or Thuy Nguye n at the address listed below, along with a letter of transmittal. **Please note that the full 9 -**  **digit Z IP**  **Code is requir**  **ed , or the mail**  **will be returned to the registrant.**

**USEPA National Pesticide Standards Repository**  **Analytical Chemistry Branch/BEAD/OPP 701 Mapes Road**  **Fort George G. Meade, MD 20755**  **- 5350**  The letter of transmittal should include the assay of the standard, name of the anal ytical method used, a statement of principal impurities, purification procedures employed, storage requirements, and special precautions for safe handling. Replacement of standards may be required periodicall y if supplies are exhausted, if the standards expire, or if decompositionMethoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 12 of 45 occurs during storage. Material Safety Data Sheets (MSDSs) must accompany all anal ytical standards as specified b y the Occupational Safety and Health Administration (OSHA) in 29CFR§1910.1200. In addition to the parent compound, 4 metabolites (included in risk assessment) are currentl y available in the NPSR, as listed below with their respective expiration dates. Methox yf enozide metabolite RH - 117236 3 September 2013 Methox yf enozide metabolite RH - 1 41518 26 July 2013 Methox yf enozide metabolite RH - 151055 15 July 2014 Methox yf enozide metabolite RH - 152,072 10 October 2010 **3. 0**  **Chemical Identity** Methox yf enozide is a diacylhydrazine insecticide used on a variety of crops for control of army worms and other lepidopterous pest species. It mimics the action of the molting hormone of lepidopterous larvae, causing the larvae to undergo an incomplete and premature molt, which ultimately

results in their death. Methoxyfenozide is currentl y registered to Dow AgroSciences. The chemical structure and nomenclature of methoxyfenozide are listed in Table 3 .1, and its physicochemical properties are presented in Table 3 .2 (below). **3.1 Nomenclature**  **TABLE 3**  **.1 Me** **thoxyfenozide Nom enclature**  . Chemical structure

Common name Methoxyfenozide Com pany experimental name RH - 2485 Molecular formula C 22 H 28N 2 O 3 Molecular weight 368.47 IUPAC name N - tert-butyl -N ′ - (3 - methoxy - o - toluoyl) - 3,5 - xylohydrazide CAS name 3 - methoxy - 2 - methylbenzoic acid 2 - (3,5 - dimethylbenzoyl) - 2 - (1,1 - dimethylethyl)hydrazide CAS registry number 161050 - 58 - 4 End - use product (EP) 2 lb ai/gal (240 g ai/L) flowable concentrate (FlC) formulation (Intrepid 2F; EPA Registration #62719 - 442).

C H 3 O N H N O C H 3

C H 3 C H 3 C H 3

O C H 3 C H 3Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 13 of 45 **3.2 Physic**  **oc hemical Characteristics**  **TABLE 3**  **.2 Physicochemical Properties of Methoxyfenozide.** 

**Param eter**  **Value Reference**  Melting point/range (oC) 206.1 - 208 D231303, H. Podall, 19 May 1997 pH 7.0 Density (g/cm 3 ) 0.740 ± 0.0081 Water solubility (mg/L at 20oC) 3.3 Solvent solubility (g/L at 20oC) N - heptane 1.87 Xylene 3.38 1,2 - dichloroethane 36.72 Methanol 192.92 2 - Propanol 50.22 Vapor pressure (Pa at 25oC) 1.33 x 10 - 5 Dissociation constant, pKa None Octanol/water partition coefficient ( Log [ KOW ] ) 3.72 ± 0.04 UV/visible absorption spectrum No absorption expected at λ> 300 nm Methox yf enozide is a solid under ambient conditions , and has a somewhat low volatility . The compound has a relatively low solubility in water, and moderate solubility i n organic solvents . Its octanol/water partition coefficient suggests that accumulation of methoxyfenozide in fatty tissues is possible . **3.3 Pesticide**  **Use Pattern/Directions for Use (860.1200)** IR- 4 has requested that new Section 3 uses of the insecticide methoxyfenozide be added to the label for Intrepid 2F (Reg istration # 62719 - 442). The proposed new uses would be on herbs (subgroup 19A) except chives, dates, sorghum and caneberries (subgroup 13 - 07A). Intrepid 2F is an FlC formulation containing 22.6% ai by weight, which is equivalent to 2 lb ai/gal . Examples of supplemental labels for Intrepid 2F were provided, and the proposed use directions therein are summarized in Table 3.3 , below . **TABLE 3.3**  **Summary of Directions for Use of Methoxyfenozide .**  **Application Type;**  **Equipment Use**  **Rate**

**(lb ai/A) Max. Uses** 

**P er Season**  **Max. Seasonal** 

**Use Rate (lb ai/A)**  **1 PHI**  **1**

**(Days) Use Directions**  **, Application Timing,** 

**and Limitations Herbs (Subgroup**  **19A) Except Chives**  Foliar; Ground and Aerial 0.12 NS **2** 1.0 1 Minimum RTI **3** of 10 days. Ground application: Apply in a minimum of 10 GPA**4** to young crop or small plants. Apply in a minimum of 20 GPA to densely foliated or difficult - to - cover crops to ensure thorough coverage. Aerial application: Apply in a minimum of 10 GPA.Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 14 of 45 **TABLE 3.3**  **Summary of Directions for Use of Methoxyfenozide .**  **Application Type;**  **Equipment Use**  **Rate**

**(lb ai/A) Max. Uses** 

**P er Season**  **Max. Seasonal** 

**Use Rate (lb ai/A)**  **1 PHI**  **1**

**(Days) Use Directions**  **, Application Timing,** 

**and Limitations Dates**  Ground (Airblast) 0.31 NS 1.0 7 Begin applications before eggs hatch. Minimum RTI of 10 days. Alternate or intersperse with other insecticides. Apply in a minimum of 100 GPA. **Sorghum** Foliar; Ground and Aerial 0.16 NS 0.75 3, 21 **5** Apply at first sign of egg hatch or when infestations reach threshold levels . Ground application: Apply in a minimum of 15 GPA. Aerial application: Apply in a minimum of 10 GPA. **Caneberries (Subgroup 13 -**  **07A)** Foliar; Ground and Aerial 0.25 3 0.75 3 Apply at initiation of egg - laying. Make second application at 100% petal fall. A third application may be required under high pest pressure. Minimum RTI of 7 days. Ground application : Apply in a minimum of 30 GPA. Aerial: Apply in a minimum of 10 GPA. 1 . PHI = Pre - Harvest Interval. 2. NS = Not Specified . 3. RTI = Re - T reatment Interval . 4. GPA = G allons Per Acre . 5. Minimum PHI of 3 days for forage and sweet sorghum stalks, and 21 days for grain and stover . Conclusions: The u se directions for application to herbs , caneberries, dates and sorghum are sufficient to allow for evaluation of the submitted residue data relative to the proposed use pattern s . **4.0 Metabolite/Degradate Residue Profile**  **4.1 Nature of the Residue**  **Me tabolism** **Assessment Review Committee (MA RC) Memo; D258034 W. Wassell; 23 July 1999**  **D251225; W. Wassell; 27 July 1999 D259989; W. Wassell; 8 August 2000**  The nature of methox yfenozide residues in primary crops is adequately understood, based on acceptable metabolism studies in cotton, apples, grapes and rice. Methoxyfenozide does not undergo extensive metabolism in primary crops. HED has determined that the residue ofMethoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 15 of 45 concern (ROC), for both the tolerance expression and risk assessment in primary crops (and drinking water) , is parent methoxyfenozide only . **D269986; M. J. Nelson; 7 August 2002** The nature of methox yfenozide residues in rotational crops i s adequatel y understood, based on acceptable metabolism studies in co nfin ed , limited field, and extensive field rotational crop studies. For enforcement purposes, the ROC for high - moisture rotational crops is the parent compound; the metabolites RH - 151,05 5, RH - 152,072, RH - 117,236, RH - 152,067, RH - 131,157 and RH - 152,071 are also to be taken into account for risk assessment. For enforcement purposes, the ROCs for low - moisture rotational crops are the combined residues of parent and metabolites RH - 151,055, RH - 152,072 and RH - 117,236; metabolites RH - 152,067, RH - 131,157 and RH - 152,071 are also to be taken into account for risk assessment. **Me tabolism** **Assessment Review Committee (MARC) Memo; D258034 W. Wassell; 23 July 1999** The nature of the residue in ruminants and poultry is adequatel y understood, based on the available metabolism studies in lactating goats , and laying hens , respectively . HED has determined that the ROC in milk and ruminant tissues (other than liver and ki dney) is parent compound; in ruminant liver and kidney it is methoxyfenozide and its RH - 141,518 metabolite. The residue of concern in poultry meat (muscle) and fat is parent methoxyfenozide. The residue of concern in eggs, poultry liver, and poultry

meat by products is methoxyfenozide and its metabolite RH - 141,518. **4.1.1 Summary of Plant**  **and /** **or Livestock**  **Metabolism (860.1300)** Data have been submitted and reviewed depicting the metabolism of methoxyfenozide in numerous crops and the environment. HED has determined the plant and livestock ROCs for purposes of tolerance enforcement and risk assessment ; see Table 4.1.1 , below . **Table 4.1.1 Summary of Methoxyfenozide Metabolites and Degradates to be included**  **in the Risk**

**Assessment and Tolerance Expression. Matrix**  **Residues Included in Risk Assessment**  **Residues Included in Tolerance Expression**  Plants Primary Crops Parent methoxyfenozide Parent methoxyfenozide

Rotational Crops (High Moisture) Parent methoxyfenozide and

metabolites, RH - 151,055, RH - 152,072, and RH - 117,236, RH - 152,067, RH 131,157 and RH - 152,071 Parent methoxyfenozide Rotational Crops (Low Moisture) Parent methoxyfenozide and

metabolites, RH - 151,055, RH - 152,072, and RH - 117,236, RH - 152,067, RH 131,157 and RH - 152,071 Parent methoxyfenozide and metabolites RH - 151,055, RH 152,072, and RH - 117,236Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 16 of 45 **Table 4.1.1 Summary of Methoxyfenozide Metabolites and Degradates to be included in the Risk** 

**Assessment and Tolerance Expression. Matrix**  **Residues Included in Risk Assessment**  **Residues Included in Tolerance Expression**  Livestock Ruminant Milk,

Meat and Fat Parent methoxyfenozide Parent methoxyfenozide Ruminant Liver and Other Meat By products Parent methoxyfenozide and metabolite

RH - 141,518 Parent methoxyfenozide and metabolite RH - 141,518 Poultry Meat and Fat Parent methoxyfenozide Parent methoxyfenozide Poultry Eggs, Liver and Other Meat By products Parent methoxyfenozide and

metabolite RH - 141,518 Parent methoxyfenozide and metabolite RH - 141,518 Drinking Water Parent methoxyfenozide Not applicable Conclusions : The nature of the residue in plants and animals has been adequately delineated. **4.1. 2**  **Summary of Confined Rotational Crops (860.l850) Me** **tabolism Assessment Review**  **Committee (MARC) Memo; D258034 W. Wassell; 23 July 1999 D251225; W. Wassell; 27 July 1999**  **D269986; M. J. Nelson; 7 August 2002** The nature of methox yfenozide residues in rotational crops is adequatel y understood, based on the availa ble confined rotational crop study . Following three soil applications of 14 C - methoxyfenozide at rates totaling 2.0 lb ai/A (1X rate) , total radioactive residues accumulated at ≥0.01 ppm in mustard, radishes and wheat planted 31, 91 and 364 day s after the last application. Methoxyfenozide was highly metabolized in rotational crops by oxidation, demethylation, and hydroxylation to non - conjugated metabolites, which were then conjugated with bi omolecules , yi elding bound residues and precursors in the sugar s ynthesis pathway . **4.1. 3**  **Summary of Rat Metabolism Risk Assessment Document**  **D388978 ; M.**  **Collantes ;**  **23 May 2012**  **(PP# 1E7842**  **)** In the rat, 14 C - radiolabeled methox yf enozide was rapidly

absorbed following gavage administration, with maximum peak plasma concentrations observed within 15 minutes of dosing. Peak plasma concentrations at 10 mg/kg ranged from 0.70 - 1.09 ppm in males , and 0.5 0 - 0.59 ppm in females, depending on the ring location of the radiolabel . At 1000 mg/kg, peak levels were 26.11 - 35.52 ppm in males , and 21.92 - 29.74 ppm in females. Plasma elimination was biphasic, with an α -phase T 1/2 of 0.2 - 0.6 h our s, and a β - phase T 1/2 of 15.2 - 3 5.6 h our s, and showed some variation with radiolabel location. The total plasma elimination rate was longer for the high dose compared to the low dose animals, suggesting metabolic pathway saturation, and the effect was more prominent in female rats. Radioactivity was extensively

distributed among tissues, with the highest concentrations at C max (0.25 hr) observed in the intestinal tract, stomach, liver and residual carcass. Enterohepatic circulation was observed.Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 17 of 45 Methox yf enozide did not show a potential for bioaccumulation. By 5 day s post - treatment, the highest levels were observed in the liver and carcass, but tissue radioactivity in all tissues was insignificant b y that time. Excretion of radiolabel was essentiall y complete by 48 h ours post dosing . Based on the minimal level of radioactivity in tissues at 72 hours, absorption was estimated to be at least 62 - 70% of the administered dose (biliary plus urinary

excretion). The major route of excretion was in the feces (86 - 97% of the administered dose ), with 5 - 13% of the dose excreted in the urine. Significant dose - or sex - dependent differences in metabolic disposition were not observed. Methox yf enozide was extensively

metabolized. The major routes of metabolism involved o–demethyl ation and oxidativ e hydrox yl ation of the A - ring phenyl and/or B - ring methyl groups, followed by glucuronic acid or sulfate conjugation. In addition to the parent compound, seven major metabolites were identified in excreta. These included RH - 131,157, RH - 141,581 and RH - 1 17,236, metabolites also identified in residues in crops and/or livestock. Up to 25 metabolites were isolated from urine, but the majority represented < 1 - 2% of the radioactive dose. Up to 16 metabolites were identified in the feces, including the parent compound, with only six containing ≥5% of the administered radiolabel. The major fecal metabolites in all groups were products of Phase I O - demethylatio n and oxidative hydrox yl ation on the A - ring and, to a lesser extent, the B - ring. Levels of excreted parent compound in the feces were greater in animals receiving 1000 mg/kg test material (30 - 39% of dose) when compared to the 10 mg/kg groups (14 - 26% of do se), consistent with saturation of absorption. In the bile, up to 24 metabolites were detected, with the primary metabolite (13 - 18% of dose) being derived b y glucuronide conjugation at the o - demethyl ated alpha ring. **4.1. 4**  **Summary of Environmental Degra dation**  **EFED Mem**  **o; D388876; K. Milians; 17 August 2011** Methox yf enozide is very persistent (T 1/2 = 1 to 3 years in soil and water), and moderatel y mobile (Koc = 219

–922 L/kg oc in various soils). It is stable to photolysis and hydrolysis, is not significantly

volatile, and degrades onl y very slowly by microbial activity . Degradates are predominantly

RH - 117 , 236 and RH - 131 , 154 , but these are onl y present at low concentrations. Because of its resistance to degradation and its mobility, methoxyfenozide has the potential to accumulate and to move off the site of application by leaching and erosion/runoff , resulting in ground - and surface - water contamination . **5.0 Residue Profile**  **5.1 Residue Analytical Methods (860.1340)**  **5.1.1 Data Collection Methods**  **MRID s**  **# 48994101**  **to -**  **04**Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 18 of 45 Basil: Samples of fresh and dried basil were analyzed for residues of methoxyfenozide using high performance liquid chromatography with tandem mass spectrometric detection (L C/MS/MS) according to a slight modification of Dow AgroScience s Method GRM: 02.25, Determination of Residues of Methoxyfenozide in High Moisture Crops by Liquid Chromatography with Tandem Mass Spectrometry Detection . This method has been assessed previously , and deemed acceptable for data gathering purposes. The petitioner used the lowest levels of method validation (LLMVs) of 0.01 and 0.05 ppm for fresh and dried samples, respectivel y, as the limits for reporting residues. The method was adequate for data collection, based on acceptable method validation and concurrent recovery data. The fortification levels used in the concurrent recoveries were adequate to bracket expected residue levels. With the exception of one sample (0.0592 ppm detected in one dried basil sample from Trial NM - 05) residues of methox yf

enozide equal to or above the LLMVs were not detected in any of the control samples. Modifications to the reference method included cleanup with hexane and dichloromethane (DCM) partition instead of solid phase (SPE) extraction, concentration by rotary evaporation instead of nitrogen blow down, and reconstitution of residues in water/acetonitrile (ACN) (7:3, v/v) containing 0.01% formic acid instead of water/ACN (7:3, v/v) containing 0.1% formic acid. Briefl y, residues of methox yf enozide were extracted from the homogenized samples with methanol/0.1 N HCl (9:1, v/v). After filtration, the filtrate was brought to known volume with methanol/0.1 N HCl (9:1, v/v) , and an aliquot of the aqueous extract was partitioned against hexane following the addition of 10% NaCl solution. The aqueous extract was then partitioned twice against DCM, and the DCM fraction was reduced to dry ness with rotary

evaporation before the sample was reconstituted in water/acetonitrile (7:3, v/v) containing 0.01% formic acid for anal ys is by

L C/MS/MS in the positive ionization mode. MS/MS detection of methoxyfenozide monitored the ion transition from m/z 369.2 →313.2. The method limit of detection (LOD) and limit of quantitation (LOQ) were calculated to be 0.00307 and 0.00921 ppm, respectivel y, in fresh basil, and 0.0163 and 0.0489 ppm, respectivel y, in dried basil. The method was adequatel y validated prior to , and in conjunction with , the anal ys is of the basil field trial samples (see Table 5.1.1.1) . **TABLE 5.1.1**  **.1 Summary of Method Validation and Concurrent Recoveries of Methoxyfenozide from** 

**Fresh and Dried Basil. Basil Matrix**  **Spike Level**

**(ppm) Sample** 

**Size (n) Recoveries**  **(%) Me**  **an ± Std.**  **Dev. (%) 1**  **Me thod Validation Recoveries**  Fresh leaves and stems 0.01 6 84, 75, 93, **69 2**  , 74, 71 78 ± 9

0.3 0 3 88, 87, 87 87 ± 1 10.0 3 86, 86, 99 90 ± 8Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 19 of 45 **TABLE 5.1.1**  **.1 Summary of Method Validation and Concurrent Recoveries of Methoxyfenozide from** 

**Fresh and Dried Basil. Basil Matrix**  **Spike Level**

**(ppm) Sample** 

**Size (n) Recoveries**  **(%) Me**  **an ± Std.**  **Dev. (%) 1**  Dried leaves and stems 0.05 6 81, 105, 104, 106, 105, 101 100 ± 10

2.0 3 92, 94, 91 92 ± 2 50.0 3 94, 95, 96 95 ± 1

**Concurrent Recoveries** Fresh leaves and stems 0.3 0 2 93 **3** , 89 91

74.9 - 75.0 3 93, 90, 91 91 ± 2 2.0 2 87, 88 88 300.0 3 96, 94, 85 92 ± 6 1. The standard deviation is not calculated for sample sizes n < 3; all statistics were calculated by study reviewer, with the exception of those at 0.01 and 0.05 ppm. 2. The value outside the acceptable range of 70 - 120% is shown in boldface type. 3. This is the average of two recoveries. Caneberries: Samples of blackberries and raspberries were anal yz ed for residues of methoxyfenozide via L C/MS/MS using a modification of Dow Agro Sciences Method GRM: 02.25 . This method has been assessed previousl y, and deemed acceptable for data gathering purposes. The petitioner used the LLMV of 0.05 ppm as the limit for reporting residues. The method was adequate for data collection , based on acceptable method validation and concurrent recovery data. The fortification levels used in the concurrent recoveries were adequate to bracket expecte d residue levels. No residues of methoxyf eno zide equal to or above the LLMV were detected in any of the control samples. The modifications made to the referenced method were minor, and included omitting use of a centrifuge to clarify

sample extracts an d using vacuum filtration; substituting a PFP phase for the SB - C 8 phase HPL C column; and adjusting the mobile phase to use ammonium acetate instead of formic acid. Briefl y, residues of methox yf enozide were extracted from the homogenized samples with methanol/0.1 N HCl (9:1, v/v). After filtration, the filtrate was brought to known volume with methanol, and an aliquot was diluted with water for clean up on an Evolute acidic basic neutral solid phase extraction cartridge. After loading the extract, the ca rtridge was dried under high vacuum, and residues were eluted with ACN. The eluate was diluted with ACN/10 mM ammonium acetate (1:1, v/v) for anal ys is by L C/MS/MS in the positive ionization mode. MS/MS detection of methoxyfenozide monitored the ion transi tion from m/z 369 →149. Based on recoveries of samples fortified at the LLMV (0.05 ppm), the method LO D and LOQ were calculated to be 0.0040 and 0.012 ppm, respectivel y. The method was adequatel y validated prior to , and in conjunction with , the anal ys is of caneberry field trial samples (see Table 5.1.1.2 ) .Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 20 of 45 **TABLE 5**  **.1 .1.2**  **Summary of Method Validation and Concurrent Recoveries of Methoxyfenozide from**

**Caneberries. Matrix**  **Spike Level (ppm)**  **Sample Size (n) Recoveries**  **(%) Me**  **an ± Std. Dev. (%) 1**  **Me thod**  **Validation Recoveries** Blackberries 0.05 3 90, 91, 89 90 ± 1

0.5 0 3 93, 91, 91 92 ± 1 5.0 3 89, 88, 91 89 ± 2

**Concurrent Recoveries** B lackberries , raspberries **2** 0.05 3 86, 85, 90 87 ± 3 Raspberries 5.0 1 92 92 1. The standard deviation is not calculated for sample sizes n < 3; all statistics were calculated by study reviewer. 2. One recovery is from a raspberry sample, and two recoveries are from blackberry samples. Dates: Date s amples were anal yz ed for residues of methoxyfenozide via LC/MS/MS using a procedure derived from Dow A groSciences Method GRM: 02.25 and Rohm and Haas Report # 34 - 98 - 87 ( Tolerance Enforcement Method for Parent RH - 2485 in Pome Fruit). The petitioner used the LLMV of 0.01 ppm as the limit for reporting residues. The method was adequate for data collection , based on acceptable method validation and concurrent recovery data. The fortification levels used in the method recoveries were adequate to bracket expect ed residue levels. No residues of methox yf enozide equal to or above the LLMVs were detected in any of the control samples. Briefl y, residues of methox yf enozide were extracted from the homogenized samples with methanol/0.1 N HCl (9:1, v:v). After filtration, the filtrate was brought to known volume with methanol, and an aliquot was diluted with water for clean up on an Evolute acidic basic neutral solid phase extraction cartridge. After loading the extract, the cartridge was dried under high vacuum, and residues were eluted with ACN. The eluate was diluted with ACN/10 mM ammonium acetate (1:1, v:v) for anal ys is by L C/MS/MS in the positive ionization mode. MS/MS detection of methoxyfenozide monitored the ion transition from m/z 369 →149. Based on recov eries of samples fortified at the LLMV (0.0 1 ppm), the method LO D and LOQ were calculated to be 0.0040 and 0.012 ppm, respectivel y. The method was validated prior to , and in conjunction with , the anal ys is of date field trial samples (see Table 5.1.1.3 ) . **TABLE 5 .1**  **.1.3 Summary of Method Validation and Concurrent Recoveries of Methoxyfenozide from** 

**Dates. Date Matrix**  **Spike Level (ppm)**  **Sample Size (n) Recoveries**  **(%) Me**  **an ± Std. Dev. (%)*** **Me thod Validation Recoveries**  Dried fruit 0.01 3 85, 84, 84 84 ± 1

1.0 3 87, 87, 89 88 ± 1 20 3 88, 86, 88 87 ± 1Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 21 of 45 **TABLE 5 .1**  **.1.3 Summary of Method Validation and Concurrent Recoveries of Methoxyfenozide from** 

**Dates. Date Matrix**  **Spike Level (ppm)**  **Sample Size (n) Recoveries**  **(%) Me**  **an ± Std. Dev. (%)*** **Concurrent Recoveries** Dried fruit 0.01 2 92, 91 92 * The standard deviation is not calculated for sample sizes n < 3; all statistics were calculated by study reviewer. Sorghum: Samples of sorghum commodities , from both the field trial and processing studies, were anal yz ed for residues of methoxyfenozide via LC /MS/MS using a slight modification of Dow AgroSciences Method GRM 02.25. For all matrices (forage and stalks, grain and stover), the petitioner used the LLMV of 0.01 ppm as the limit for reporting residues. The method was adequate for data collection , based on acceptable method validation and concurrent recovery data. The fortification levels used in the concurrent recoveries were adequate to bracket expected residue levels. No residues of methox yf eno zide equal to or above the LLMV were detected in any control samples. Briefl y, residues of methox yf enozide were extracted from the homogenized samples with methanol/ 0 .1 N HCl (9:1 , v: v). After filtration, the filtrate was brought to known volume with methanol, and an aliquot was diluted with water for clean up on an Evolute acidic basic neutral solid phase extraction cartridge; after loading the extract, the cartridge was dried under high vacuum, and residues were eluted with ACN. The eluate was diluted with ACN/10 mM ammonium acetate (1:1, v:v) for anal ys is by L C/MS/MS in the positive ionization mode. MS/MS detection of methoxyfenozide monitored the ion transition fro m m/z 369 →149. The method LOD and LOQ , respectivel y, were calculated to be 0.00711 and 0.02134 ppm in sorghum forage/ stalks, 0.00125 and 0.00374 ppm in sorghum grain, 0.00263 and 0.00790 in sorghum stover , 0.00064 and 0.00191 in AGF, and 0.00028 and 0.00083 in sy rup . The LLMV for all sorghum matrices was 0.01 ppm. The method was validated prior to , and in conjunction with , the anal ys is of sorghum field trial and processing study samples (see Table 5.1.1. 4 ) . **TABLE 5 .1**  **.1.4 Summary of Method Validat**  **ion and Concurrent Recoveries of Methoxyfenozide from**

**Sorghum Commodities. Sorghum Matrix**  **Spike Level (ppm)**  **Sample Size (n) Recoveries**  **(%) Me**  **an ± Std. Dev. (%) 1**  **Me thod Validation Recoveries**  Forage 0.01 3 88, 85, **131 2**  101  26

0.1 0 3 85, 86, 83 85  2 1.0 3 86, 85, 85 85  1 10 3 85, 86, 79 83  4 Grain 0.01 3 88, 85, 83 85  3

0.1 0 3 84, 85, 85 85  1 1.0 3 87, 86, 86 86  1 Stover 0.01 3 75, 72, 75 74  2

0.1 0 3 80, 77, 78 78  2 1.0 3 80, 82, 82 81  1Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 22 of 45 **TABLE 5 .1**  **.1.4 Summary of Method Validat**  **ion and Concurrent Recoveries of Methoxyfenozide from**

**Sorghum Commodities. Sorghum Matrix**  **Spike Level (ppm)**  **Sample Size (n) Recoveries**  **(%) Me**  **an ± Std. Dev. (%) 1**  **Concurrent Recoveries** Forage 0.01 3 75, 77, 78 77  2

0.1 0 3 83, 83 83 10 3 87, 88, 89 88  1 Stalks 0.1 0 1 86 86 Grain 0.01 2 88, 78 83

0.1 0 1 87 87 1.0 1 89 89 5.0 3 89, 88, 89 89  1 Stover 0.01 2 **60 2**  , **57 2**  59

1.0 1 90 90 20 4 86, 86, 87, 90 87  2 1. The standard deviation is not calculated for sample sizes n < 3; all statistics were calculated by the study revie wer. 2. Values outside the range of 70 - 120% are shown in boldface type. Conclusions: Adequate method validation data have been submitted for the LC /MS/MS method used for the determination of methoxyfenozide residues in the various commodities . No additional data are required in support of this data collection method. **5.1.2 Multi**  **- Residu**  **e Methods (860.1360) D**  **249438, D**  **249458, D**  **251218 & D**  **251225 ;**  **W. Wassell ;**  **27 July 1999** Data concerning the recovery of methox yf

enozide using the FDA multiresidue method protocols ( PAM Volume I

) were previously

submitted to, and reviewed by , HED. Methoxyfenozide was not recoverable b y any of these procedures. The data were forwarded to FDA for evaluation, and the updating of PAM Volume I . **5.1.3 Tolerance Enforcement Methods**  **D358341 ;**  **D .**  **Rate ;**  **10 June**  **2009** Several HPLC/UV and HPL C/MS methods are available for enforcing tolerances of methoxyfenozide in primary crops , Method TR 34 - 96 - 88 , Method TR 34 - 98 - 87 , Method TR 34

– 00 - 38 , Method TR 34 - 00 - 107 , Method TR 34 - 00 - 109, and Method TR 34 - 99 - 7 4 . Adequate method validation, radio - validation, and independent laboratory validation (ILV) data have been provided for these methods. Successful petition method validation (PMV) trials were conducted on Methods TR 34 - 96 - 88 and TR 34 - 98 - 87, and the Biol ogical and Economic Anal ys is Division’s (BEAD’s) Analy tical Chemistry

Branch (ACB) concluded that PMV trials were not required for the other methods , s ince they are similar to the validated methods. For each of these methods, residues of methoxyf enozide are extracted with acidic aqueous methanol, filtered , and diluted with 10% sodium chloride. Extracts are then purified by sequential liquid - liquid partitioning with hexane and dichloromethane (DCM). Residues in theMethoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 23 of 45 DCM fraction are further purified b y e lution through one or more of the following column types: basic alumina, silica gel, carbon, Florisil, or C 18 . Residues in the final eluate are concentrated, re - dissolved in ACN/water, and anal yz ed b y reverse -phase HPL C using UV (240 nm) or MS (m/z 367) with external standards. The LOQ for methoxyf enozide is 0.01 - 0.05 ppm , depending on the plant commodity . An adequate enforcement method is also available for determining the ROCs in rotated crops. Method TR 34 - 00 - 41 includes an HPL C/UV method that det ermines methoxyfenozide residues in high - moisture rotational crops , and an HPL C/MS method that determine s residues of methoxyfenozide and its metabolites RH - 117,236, RH - 151,055 and RH - 152,072 (determined as RH - 151,055) in low - moisture rotational crops. Adequate method validation, radio - validation, and ILV data have been submitted for this method, and ACB concluded that a PMV trial was not needed for this method owing to its similarity to Method TR 34 - 98 - 87. **5.2 Storage Stability (860.1380)**  **MRIDs #48994101 to -**  **04** Basil: Sample storage conditions and durations are reported in Table 5.2.1 , below . Samples of basil leaves and stems (both fresh and dried) were stored frozen ( - 37 to - 0.6°C), from sampling to extraction, for 735 - 806 days (24.1 - 26.5 months) and 735 - 805 days (24.1 - 26.4 months), respectivel y. Samples were anal yz ed within 0 - 4 days of extraction. To support the sample storage durations , a concurrent storage stability study was conducted with the field trial study ; the results are presented in Table 5 .2.2 , below . Stability during frozen storage was evaluated after intervals of 760 and 758 day s in fresh basil and dried basil, respectively . The data demonstrate that residues of methox yfenozide were stable in the fresh and dried basil samples for intervals of up to 760 and 758 day s (25.0 and 24.9 months) of frozen storage, respectivel y. Zero day data were not provided; IR- 4 is reminded that storage stability studies should always include a 0 - day sampling interval to establish the residue levels present at the time samples are placed into storage (see OCSPP 860.1380[d][6][i]). Although the storage interval tested in the concurrent storage stability study is less than the maximum storage duration of the field trial samples, it is 94% as long as the longest actual storage duration. These data are adequate to support the storage conditions and durations of the basil samples from the submitted field trials. **TABLE 5**  **.2.1 Summary of Storage Conditions.**  **Basil Matrix Storage** 

**Temperature (°C)**  **Actual Storage Duration 1**  **(Days [Months]) Interval of Dem**  **onstrated Storage Stability**  **2 (Days [Months])**  Fresh leaves and stems - 37 to - 0.6 735 - 806 [ 24.1 - 26.5 ] 760 [ 25.0 ] Dried leaves and stems 735 - 805 [ 24.1 - 26.4 ] 758 [ 24.9 ] 1. Duration from sampling to extraction. Samples were analyzed within 0 - 4 days of extraction. 2. Based on concurrent storage stability study. See Table C.2.2 (below) .Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 24 of 45 **TABLE 5 .2.2**  **Stability of Methoxyfenozide in Basil Matrices. Basil Matrix**  **Spike**

**Level (ppm)**  **Storage**

**I nterval**  **1 (** **D ays)**  **Fresh**

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

**Residues (%) Me**  **an**

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

**R ecovery**  **(%) 2**  Fresh leaves and stems 1.0 760 85.9 92. 5 , 91.6, 92.0 92. 0 107.1 Dried leaves and stems 1.0 758 87.6 83. 0 , 83.1, 83.7 83.3 95.1 1. Interval from fortification to extraction. Samples were analyzed on the day of extraction. 2. Corrected for the recovery in a freshly fortified sample; calculated by the study revie wer. Caneberries: Sample storage conditions and durations are reported in Table 5 .2 .3 , below . Berry samples were stored frozen ( - 20°C) , from sampling to extraction for anal ys is , for 130 - 189 day s (4.3 - 6.2 months). Samples were anal yz ed within 0 - 1 days of extraction. No st orage stability data were provided. Samples for a concurrent storage stability study were prepared; however, they were not anal yz ed because the protocol stated that anal ys is of these samples would be required onl y in the event of a freezer failure. Existing storage stability data indicate that methoxyfenozide is stable at ≤ - 20°C for intervals of up 629 day s in citrus fruits (D396397 ; W. T. Drew; 2 March 2 0 12). In addition, freezer storage stability has been demonstrated for a period of at least 12 months in 5 diverse crops, including cottonseed (PMRA #586719), field corn grain (PMRA # 586721), head lettuce (PMRA # 58 6722), sugar beet roots (PMRA #1843187), and tomatoes (PMRA # 586720). These data are adequate to support the storage conditions and durations o f the caneberry samples from the submitted field trials . **TABLE 5**  **.2 .3**  **Summary of Storage Conditions. Matrix**  **Storage**

**Temperature (°C)**  **Actual Storage Duration 1**  **(D ays**  **[M onths**  **] )**  **Interval of Dem onstrated Storage**  **Stability 2**  **(Days [Months])** Caneb erries - 20 130 - 189 [ 4.3 - 6.2 ] 629 [20.6] 1. Duration from sampling to extraction. Samples were analyzed within 0 - 1 days of extraction. 2. In citrus fruit (r efer to D396397 ; W. T. Drew ; 2 March 20 12 ) . Dates: Sample storage conditions and durations are reported in Table 5.2.4, below. Samples of dates were stored frozen ( - 20°C), from sampling to extraction for anal ys is, for 104 - 131 days (3.4 - 4.3 months). Samples were anal yz ed on the day of extraction. To supp ort the sample storage durations , a concurrent storage stability study was conducted with the field trial study ; the results are presented in Table 5.2.5, below. Stability during frozen storage was evaluated after an interval of 118 days. The data demons trate that residues of methoxyfenozide were stable in date samples for intervals of up to 118 day s (3.9 months) of frozen storage. Zero - day data were not provided; IR - 4 is reminded that storage stability studies should alway s include a 0 - day sampling interval to establish the residue levels present at the time samples are placed into storage (see OCSPP Residue Chemistry Test Guideline 860.1380[d][6][i]). Although the storage interval tested in the concurrent storage stability study is less than the maximum storage duration of field trial samples, it is 90% as long as the longest actual storage duration. These data are adequate to support the storage conditions and durations of date samples from the submitted field trials.Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 25 of 45 **TABLE 5**  **.2. 4**  **Summary of Storage Conditions.**  **Date Matrix Storage Tem** **perature (°C)**  **Actual Storage Duration 1** 

**(Days [M onths**  **] )**  **Interval of Dem onstrated Storage**  **Stability 2**  **(Days [Months])** Dried fruit - 20 104 - 131 **3** [ 3.4 - 4.3 ] 118 [ 3.9 ] 1. Duraton from sampling to extraction. Samples were analyzed on the day of extraction. 2. Based on concurrent storage stability study. See Table 5 .2. 5 , below . 3. One of the control samples was not extracted until after 157 days of storage; all other control samples were extracted after 104 - 111 days of storage. **TABLE 5.2.5 Stability of Methoxyfenozide in Dates (Dried Fruit).**  **Date Matrix**  **Spike**

**Level (ppm)**  **Storage Interval**  **1 (Days**  **[M onths])**  **Procedural Recoveries**

**[M ean] (%)**  **2 Recovered Residues**  **(%) Me**  **an**

**Recovery (%)**  **2 Corrected** 

**Recovery (%)**  **3** Dried fruit 1.0 118 87, 88, 81 [85] 0.843, 0.807, 0.884 84 99 1. Interval from fortification to extraction. Samples were analyzed on the day of extraction. 2. Calculated by study reviewer. 3. Corrected for mean recovery in freshly fortified samples; calculated by the study revie wer. Sorghum: Sample storage conditions and durations are reported in Table 5 .2. 6 , below . Samples of sorghum forage, stalks, grain and stover were stored frozen ( - 20°C) , from collection to extraction, for 573 - 640 days (18.8 - 21.0 months), 564 - 609 days (18.5 - 20.0 months), and 557 - 596 days (18.3 - 19.6 months), respectivel y. Samples were anal yz ed within 0 - 3 days of extraction. To support the sample storage durations , a concurrent storage stability study was conducted with the field trial study ; the results are presented in Table 5 .2. 7 , belo w . Stability during frozen storage was evaluated after intervals of 607, 598 and 599 day s in forage , grain and stover, respectivel y. The data demonstrate d that residues of methoxyfenozide were st able in the forage , grain and stover samples for intervals of up to 607, 598 and 599 day s (19.9, 19.6 and 19.7 months), respectivel y. Zero - day

data were not provided; IR - 4 is reminded that storage stability studies should always include a 0 - day sampling interval to establish the residue levels present at the time samples are placed into storage (see OCSPP 860.1380[ d][ 6 ][i ] ) . Although the storage intervals tested in the concurrent storage stability study are less than the maximum storage durations of field trial samples for forage/ stalks and grain, they are ≥ 95% a s long as the longest actual storage duration. These data are adequate to support the storage conditions and durations of samples from the submitted sorghum field trials. **TABLE 5**  **.2. 6**  **Summary of Storage Conditions. Sorghum**  **Matrix Storage** 

**Temperature (°C)**  **Actual Storage Duration 1**  **(Days [Months]) Interval of Dem**  **onstrated Storage Stability**  **2 (Days [Months])**  Forage/stalks - 20 573 - 640 [ 18.8 - 21.0 ] 607 [ 19.9 ] Grain 564 - 609 [ 18.5 - 20.0 ] 598 [ 19.6 ] Stover 557 - 596 18.3 - 19.6 ] 599 [ 19.7 ] 1. Duration from sampling to extraction. Samples were analyzed within 0 - 3 days of extraction. 2. Based on concurrent storage stability study. See Table 5 .2. 7 , below .Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 26 of 45 **TABLE 5.2.7 Stability of Methoxyfenozide in Sorghum Matrices.**  **Sorghum Matrix**  **Spike Level**

**(ppm) Storage** 

**I nterval**  **1 (** **D ays)**  **Fresh Fortification**

**Recoveries [Average 2**  **] (%)**  **Recovered**

**Residues (%) Me**  **an**

**Recovery 2**  **(%) Corrected** 

**R ecovery**  **3 (%)**  Forage 1.0 607 89.7, 89.2, 86.1 [88.3] 85.7, 86.8, 86.0 86.2 97.5 Grain 1.0 598 85.5, 85.0, 85.6 [85.4] 79.3, 80.7, 79.4 79.8 93.5 Stover 1.0 599 84.1, 81.5, 83.9 [83.2] 83.7, 82.2, 85.2 83.7 100.6 1. Interval from fortification to extraction. Samples were analyzed on the day of extraction. 2. Calculated by the study reviewer. 3. Corrected for mean recovery in freshly fortified samples; calculated by the study revie wer. Conclusions : There are no storage stability issues, and no corrections for potential decline during storage are needed in reviewing the residue studies submitted for the various commodities . **5.3 Residue Data**  **5.3.1 Crop Field Trials (860.1500)**  **MRIDs #48994101 to -**  **04** Basil: IR- 4 submitted field trial data for methoxyfenozide on basil. A total of 5 crop field trials were conducted in the US and Canada during the 2009 growing season in NAFTA Growing Zones 2 (NC), 3 (FL), 5A (WI), 9 (NM) and 12 (BC). Each trial consisted of one untreated (control) plot, and one plot treated with an FlC formulation of methox yfenozide (Intrepid 2F) containing 2 lb ai/gal . The treated plots received 4 foliar directed or broadcast applications of the FlC formulation at rates of 0.242 - 0.261 lb ai/A per application, with RTI s of 9 - 11 day s, for total application rates of 0.988 - 1.032 lb ai/A. Applications were made using backpack sprayers, in spray volumes of 21 - 4 3 GPA of water, using a non - ionic surfactant (NIS) as an adjuvant (0.25 - 0.50% v/v). Samples of mature fresh basil (stems and leaves) were harvested at a PHI of 1 day at all trial sites. At each trial site, additional samples were collected at a 1 - day PHI , and dried (in a drying oven or forced - air dryer) for 1 - 7 days to generate dried basil (stems and leaves). At one field trial, fresh basil was harvested at PHI s of 1, 3, 6 and 12 day s to assess residue decline. Following 4 foliar directed or broadcast applications of methoxyfenozide to basil at total rates of 0.988 - 1.032 lb ai/A, residues (and per- trial averages) of methoxyfenozide were 9.26 - 47.2 (9.88 - 43.4) ppm in fresh basil, and 56.3 - 194 (60.5 - 188) ppm in dried basil harvested at a 1 - day PHI (see Ta ble 5.3.1.1 , below ). As noted previousl y in Section 5.1.1, one control sample at Trial NM - 05 had a residue of 0.0592 ppm, which exceeded the LLMV. However, the residues observed in the trial far exceeded this residue; therefore, this control sample had minimal to no impact on the final residue v alues summarized below. In the residue decline trial, the per - trialMethoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 27 of 45 average residues at PHIs of 1, 3, 6 and 12 day s were 43.4, 14.3, 11.5 and 0.823 ppm, respectivel y, which demonstrated that residues decreased with longer PHIs. **TABLE 5.3.1.1**  **Summary of Residue Data from** **Basil Field Trials with Methoxyfenozide. Basil**  **Comm odity**  **Total Use**

**Rate (**  **lb ai/A)**  **[g ai/ha] PHI** 

**(Days) Residue Levels**  **( ppm** **) 1** 

**n Min.**  **Max. LAFT**  **2 HAFT**  **2 Median**  **Me an**  **Std. Dev.** Fresh leaves and stems 0.988 - 1.032

[1107 - 1157] 1 10 9.26 47.2 -- -- 19.2 21.7 12. 3 5 -- -- 9.88 43.4 19.2 21.7 12.8 Dried leaves and stems 10 56.3 194 -- -- 10 0 110 44.8 5 -- -- 60.5 188 102 110 47.0 1. For n = 5 , values reflect per - trial averages; for n = 10, values reflect statistics for individual samples . 2. LAFT = Lowest Average Field Trial; HAFT = Highest Average Field Trial. Caneberries: IR- 4 submitted field trial data for methoxyfenozide on caneberry . A total of 6 crop field trials on caneberry were conducted in the US during the 2010 growing season in NAFTA Growing Zones 2 (NC, blackberry), 5A (MI , blackberry), 10 (CA, blackberry) and 12 (OR, one trial on blackberry , and two trials on raspberry). Examination of the field trial records indicates that one Field Research Director (FRD) su pervised all 3 field trials at one city in OR. Nonetheless, each trial in OR constitutes a separate trial for purposes of OCSPP Residue Chemistry

Test Guideline 860.1500 data requirements because of sufficient differences in their residue levels . In addition, these trials differed with regard to spray volumes and crops ( 2 raspberry , 1 blackberry). Each trial consisted of one untreated (control) plot , and one plot treated with Intrepid 2F . The treated plots received 3 foliar directed applications of Intrepid 2F at rates of 0.244 - 0.261 lb ai/A per application , with RTIs of 6 - 8 days , for total application rates of 0.744 - 0.778 lb ai/A. Applications were made using backpack sprayers , in spray volumes of 30.85 - 86.26 GPA of water, using an NI S as an adjuv ant (0.01 - 0.13% v/v) . Samples of berries were harvested at a PHIof 3 day s at all trial sites . At one field trial, berries were harvested at PHI s of 1, 3, 6 and 13 days to assess residue decline. Following 3 foliar directed applications of methoxyfenozide to caneberries at total rates of 0.744 - 0.778 lb ai/A , residues (and per- trial averages) of metho x yf enozide were 0.62 - 2.5 (0.68 - 2.5) ppm in berries that were harvested at a 3 - day PHI (see Table 5.3.1. 2, below) . At the residue decline trial, the per- trial average residues at PHI s of 1, 3, 6 and 13 day s were 2.3, 2.2, 1.8 and 1.6 ppm, respectivel y, which demonstrated that residues decrease with longer PHIs.Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 28 of 45 **TABLE 5.3.1.2**  **Summary of Residue Data from Caneberry Field Trials with Methoxyfenozide.**  **Comm odity**  **Total Use** 

**Rate (lb**  **ai/A) [g ai/ha]**  **PHI**

**( D**  **ays) Residue Levels**  **( ppm** **) 1** 

**n Min.**  **Max. LAFT**  **2 HAFT**  **2 Median**  **Me an**  **Std. Dev.** Caneb erries 0.744 - 0.778

[834 - 872] 3 12 **1** 0.62 2.5 -- -- 1. 90 1.70 0.6 5

6 **1**

-- -- 0.68 2. 5 1.90 1.73 0.67 1. For n = 6 , values reflect per - trial averages; for n = 12, values reflect statistics for individual samples. S tatistics were calculated by the study reviewer. 2. LAFT = L owest Average F ield Trial; HAFT = H ighest Average Field T rial. Dates: IR- 4 submitted field trial data for methoxyfenozide on dates. A total of 3 crop field trials on dates were conducted in the US during the 2010 growing season in NAFTA Growing Zone 10 (CA). Examination of the field trial records indicates that one Field Research Director (FRD) supervised 4 trials (all trials in the study), which were within approxi mately 10 miles of each other. For purposes of OCSPP Residue Chemistry Test Guideline 860.1500 data requirements, the Trials 10 - CA2 2 and 10 - CA23 are considered replicates of the same trial. The other two trials are considered sufficiently different from this replicate pair , and from each other , to be considered separate trials. The 3 trials (including one replicate pair) are considered separate trials because of sufficient differences in locations, crop varieties, and/or spray concentrations. Each trial consisted of one untreated (control) plot , and one plot treated with Intrepid 2F. Each plot consisted of 6 trees. The treated plots received 3 foliar directed applications of Intrepid 2F at rates of 0.096 - 0.313 lb ai/A per application , with RTI s of 9 - 11 day s , for total application rates of 0.501 - 0.933 lb ai/A. Applicatio ns were made using skid pump sprayers , in spray volumes of 64.65 - 291 GP A of water, using an NI S, or a combined vegetable oil concentrate and si licone surfactant, as an adjuvant. The first 2 applications at one trial , and the first application at another trial , used substantially

lower application rates , reflecting application of the test substance at a rate proportional to 0.31 lb ai/A, directed to the fruit bunches to runoff. An amendment to the protocol was made to specify an application rate of 0.31 lb ai/A as a spray directed to the tree canop y, wetting the fruit bunches to runoff. All remaining applications in all trials were made according to this amendment. The amendment was necessitated b y the determination that the number of date bunches in the plots was lower than normal, which resulted in much less spray being applied than the target rate. Mature date fruit was harvested at a PHI of 7 days at all trials . Following 3 foliar directed applications of methoxyfenozide at total rates of 0.501 - 0.933 lb ai/A, residues (and per- trial averages) of methox yf enozide were 1.5 - 3.3 (1.6 - 3.1) ppm in dry fruit harvested at a 7 - day

PHI (see Table 5.3.1. 3 , below) . There was no residue decline study ; however, none is needed for crops such as this that require fewer than 5 total field trials.Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 29 of 45 **TABLE 5.3.1.3**  **Summary of Residue Data from Date Field Trials with Methoxyfenozide.**  **Date Comm**  **odity Total Use** 

**Rate (lb ai/A)**  **PHI**

**(Days) Residue Levels**  **( ppm** **) 1**  **n Min.**  **Max. LAFT**  **2 HAFT**  **2 Median**  **Me an**  **Std. Dev.** Dried fruit 0.501 - 0.933 7 8 1.5 3.3 1.6 2. 3 2.0 2.0 0. 7 0 1. Except for the mi nimum and maximum , values reflect per - trial averages; n = num ber of field trials; statistics were calculated by the study revie wer. 2. LAFT = L owest Average F ield Trial; HAFT = Highest Average F ield T rial. 3. The number of trials equals 3 instead of 4 because trial pair 10 - CA2 2 /10 - CA23 constitutes a single trial with replicate samples ( for purposes of OCSPP 860.1500 data requirements ) . Sorghum: IR - 4 submi tted field trial data for methoxyf enozide on sorghum. A total of 12 crop field trials on grain sorghum were conducted in the US during the 2009 growing season in NAFTA Growing Zones 2 (NC), 4 (AR), 5 (ND 3 trials ; SD 1 trial), 6 (TX, 2 trials), 7 (NE), 8 (TX) and 10 (NM, 2 trials). There was also 1 crop field trial on sweet sorghum conducted in Growing Zone 6 (TX) during the same growing season. Examination of the field trial records indicates that one Field Research Director ( FRD ) supervised three trial s in ND, another supervised 4 trials in TX, and another supervised 2 trials in NM, with the trials in all three sets being close to each other, with the exception of one trial in TX. For purposes of OCSPP Residue Chemistry

Test Guideline 860.1500 data requirements, the trials in all three sets are considered to be separate because of sufficient differences in their residue levels for at least one of the sorghum commodities . In addition there were differences between trials in some of the sets regarding crop variety, adjuvant class , application spray volume, and irrigation ty pe . Each trial consisted of one untreated (control) plot , and one plot treated with Intrepid 2F . The treated plots received 4 foliar broadcast (11 trials) or foliar directed (2 trials) applications of Intrepid 2F at rates of 0.117 - 0.127 lb ai/A per application , with RTI s of 9 - 14 day s , for total application rates of 0.478 - 0.494 lb ai/A. Applications were made using ground equipment with CO 2 or compressed air as the propellant , in spray volumes of 8 - 49 GPA of water, using an NI S or a crop oil concentrate (COC) as an adjuvant . In the grain sorghum trials, forage was harvested at PHI s of 2 - 4 days; grain was harvested at PHIs of 11 days (one trial only) or 21 - 23 day s , and was allowed to dry

for 0 - 5 days prior to collection ; and stover was harvested at PHI s of 21 - 23 days , and was allowed to dry for 1 - 9 days prior to collection. In one field trial, additional samples of forage were harvested at PHI s of 0, 7, 11 and 14 day s to assess res idue decline. In the sweet sorghum trial, stalks were harvested at a PHIof 3 day s. Following 4 foliar broadcast or directed applications of methoxyfenozide to grain sorghum at total rates of 0.478 - 0.494 lb ai/A, residues (and per- trial averages) of metho x yf enozide were 0.70 - 5.6 (0.77 - 5.0) ppm in sorghum forage harvested at a PHI of 2 - 4 days , 0.15 - 2.6 (0.15 - 2.3) ppm in sorghum grain harvested at a PHI of 11 - 23 day s , and 0.29 - 9.7 (0.45 - 7.6) ppm in sorghum stover harvested at a PHI of 21 - 23 day s (see Table 5.3.1. 4 , below) . Following 4 foliar broadcast applications of methoxyfenozide to sweet sorghum (only 1 trial) at a total rate of 0.481 lb ai/A, residues (and per- trial average) of metho x yf enozide were 0.045 - 0.18 (0.11) ppm in sorghum stalks harvested at a PHI of 3 day s. In the residue decline trial, the per- trial average residues inMethoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 30 of 45 grain sorghum forage harvested at PHIs of 0, 4, 7, 11 and 14 day s were 6.2, 4.5, 2.6, 3.6 and 2.6 ppm , which demonstrated a residue decline during the first 7 days , with no further decline. **TABLE 5.3.1 .4**  **Summary of Residue Data from Sorghum Field Trials with Methoxyfenozide.**  **Sorghum Matrix**  **Total Use**

**Rate (lb ai/A)**  **PHI**

**(Days) Residue Levels**  **( ppm** **) 1** 

**n Min.**  **Max. LAFT**  **2 HAFT**  **2 Median**  **Me an**  **Std. Dev. 3**  **Grain Sorghum** Forage 0.478 - 0.494 2 - 4 12 0.70 5.6 0.77 5.0 2.15 2.76 1.45 Grain 11; 21 - 23 12 0.15 2.6 0.15 2.3 0.40 0.72 0.72 Stover 21 - 23 12 0.29 9.7 0.45 7.6 2.95 3.18 2.39 **Sweet Sorghum** Stalks 0.481 3 1 0.045 0.18 0.11 0.11 0.11 0.11 NA 1. Except for the minimum and maximum, values reflect per - trial averages; n = number of field trials. 2. LAFT = Lowest Average Field Trial; HAFT = Highest Average Field Trial. 3. NA = Not Applicable (the standard deviation is not calculated for sample sizes n < 3). Conclusions : The submitted crop field trial data are adequate , and support the establ ishment of permanent tolerance s in the various basil , caneberry , date and sorghum commodities, as listed in Table 6.0 (see Section 6.0) . **5.3.2 Field**  **Rotational Crops (860.1900)** Label directions for methoxyfenozide (Intrepid 2F) currently specify that crops with registered uses may be replanted at any

time, and all other food or feed crops may be replanted 7 days after the last application. Adequate l imited and extensive rotational crop field trials are available that support these rotational crop restrictions. Because the maximum seasonal use rate being proposed for date s and herbs (1.0 lb ai/A) is the same as for other registered field and vegetab le crops, no changes are required in the current rotational crop restrictions. The petitioner has proposed inadvertent tolerances in oilseed crops (the r apeseed subgroup 20A , and the s unflower subgroup 20B ) , based upon HED 's review of existing rotational crop data , and subsequent Agency

recommendations. **5.3.3 Processed Food and Feed (860.1520)**  **MRIDs #48994102** IR- 4 submitted a processing study for methox yf

enozide on grain sorghum and sweet sorghum. Two sorghum field trials were conducted in NAFTA Growing Zones 6 (TX; sweet sorghum) and 7 (NE; grain sorghum) during the 2009 growing season . At these trials , Intrepid 2F was applied to sorghum as 4 foliar broadcast applications at rates of 0.119 - 0.121 lb ai/A per application, with RTI s of 9 - 11 day s, for a total application rate of 0.481 lb ai/A. Applications were made usingMethoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 31 of 45 ground equipment (boom sprayers), in a spray volume of 15 - 21 GPA of water, containing an NI S as an adjuvant. Bulk samples of the RAC s, sweet sorghum stalks , and sorghum grain, were collec ted at PHIs of 3 and 21 day s, respectively . The RACs were processed within 56 - 80 day s of harvest into sorghum AGF , and sweet sorghum s yrup , using simulated commercial procedures. Samples of sorghum stalks and grain, and the processed sorghum commodities, were anal yz ed for residues of methox yf

enozide via LC /MS/MS using a slight modification of Dow AgroSciences Method GRM 02.25. The petitioner used the LLMV of 0.01 ppm as the limit for reporting residues of methoxyfenozide in sorghum commodities. The method was adequate for data collection, based on acceptable method validation and concurrent recovery data. No residues of methox yf

enozide equal to or above the LLMV were detected in any control samples. Samples of sorghum s talks and grain were stored frozen, from harvest to extraction, for 21.0 and 19.4 months, respectively . Samples of sorghum AGF and s yrup were stored frozen from collection until extraction, for 16.7 and 18.4 months, respectivel y. Samples were anal yz ed on the day of extraction. Storage stability data generated concurrentl y with the study demonstrated that residues of methox yf enozide were stable in sorghum forage, grain, AGF and s yrup for up to 19.9, 19.6, 17.3 and 18.4 months), respectivel y. Although the storage interval for forage tested in the concurrent storage stability study is shorter than the storage duration for stalks in the processing study , it is 95% as long as the actual storage duration. These data are adequate to support the storage conditio ns and durations of samples from the submitted sorghum processing study . Residues of methox yfenozide were 1.1 and 0.48 ppm in sorghum stalks and grain (RACs) harvested at PHI s of 3 and 21 days, respectively , following the last of 4 foliar broadcast appl ications of Intrepid 2F at a total rate of 0.481 lb ai/A. Residues of methoxyfenozide were 1.1 and 17 ppm in sorghum sy rup and sorghum AGF, respectivel y (see Table 5.3. 3 , below) . These data indicate that methoxyfenozide did not concentrate in sweet sorghum s yrup (1 X processing factor) , but did concentrate in sorghum AGF (35 X processing factor) . A maximum theoretical concentration factor for sorghum is not provided in OCSPP Residue Chemistry

Test Guideline 860.1520. **TABLE 5.3**  **.3 Residue Data from**  **Sorghum Processing Study with Methoxyfenozide. Sorghum Commodity**  **Total Rate (lb ai/A)** **PHI* (Days)** **Residues (ppm )**  **Processing Factor** Stalk (RAC) 0.481 3 1.1 -- Sy rup 1.1 1 X Grain (RAC) 0.481 21 0.48 -- AGF 17 35 X * PHI = P re - Harvest Interval.Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 32 of 45 Conclusions: The submitted sorghum processing study data are adequate, and support a tolerance of 120 ppm in ( sorghum) AGF. This will be reflected in an increase of the currentl y established tolerance in AGF, from 2.0 to 120 ppm. A tolerance in sweet sorghum s yrup is not required. **5.3.4 Meat, Milk, Poultry and Eggs (860.1480)**  No livestock feeding studies were submitted with this petition. Previously , the m aximum reasonabl y balanced dietary ( MRBD) burdens of methoxyfenozide to livestock were estimated by HED to be 35 ppm for beef cattle, 54 ppm for dairy cattle, 7.7 ppm for poultry , and 0. 2 ppm for swine. Because the proposed tolerances for this action include an increase of the tolerance in sorghum grain, the projected MRBD burdens have been reassessed. The revised values were determined to be 38 ppm for beef cattle, 55 ppm for dairy cattle, 12 ppm for poultry , and 5 ppm for swine. The revised dietary burdens are presented in Table 5.3.4 (below). These estimated dietary burdens result in anticipated residues that do not exceed the tolerances that are currentl y established in livestock commodities. **TABLE 5.3.4 Calculation of Maxim** **um Reasonably Balanced Dietary Burdens of Methoxyfenozide** 

**Residues to Livestock. Feedstuff**  **Type 1**  **% Dry Matter**  **2 % Diet**  **2 Established**  **Tolerance (ppm) Dietary Contribution**  **(ppm) 3**  **Beef Cattle** Alfalfa hay R 89 15 150 25.28 F ield c orn grain CC 88 3 5 0.05 0.0 20 Soy bean AGF CC 85 5 160 9.412 Sorghum grain CC 86 40 6.0 2.790 Soy bean seed PC 89 5 1.00 0.056 TO TAL BURDEN -- -- 100 -- **3 7.6**  **Dairy Cattle** Grass forage R 25 25 18 18.00 Alfalfa hay R 35 20 150 33.71 Sorghum grain CC 8 6 4 5 6.0 3.135 Undelinted c otton seed PC 88 10 2.00 0.227 TO TAL BURDEN -- -- 100 -- **55. 1**  **Poultry** Sorghum grain CC 8 6 75 6.0 4.500 Alfalfa meal **4** PC 89 5 150 7.50 0 Soy bean meal **4** PC 92 20 1.00 0.200 TO TAL BURDEN -- -- 100 -- **12.2**Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 33 of 45 **TABLE 5.3.4 Calculation of Maxim** **um Reasonably Balanced Dietary Burdens of Methoxyfenozide** 

**Residues to Livestock. Feedstuff**  **Type 1**  **% Dry Matter**  **2 % Diet**  **2 Established**  **Tolerance (ppm) Dietary Contribution**  **(ppm) 3**  **Swine** Sorghum grain CC 8 6 80 6.0 4.800 Field corn grain CC 88 5 0.05 0.043 Soy bean meal 4 PC 92 15 1.00 0.150 TO TAL BURDEN -- -- 100 -- **4.9 9**  1. R = Roughage; CC = Carbohydrate Concentrate; PC = Protein Concentrate. 2. OCSPP Residue Chemistry Test Guideline 860.1000 Table 1 Feedstuffs (30 June 2008). 3. Contribution = ([tolerance /% DM] X % diet) for beef and dairy cattle; contribution = ([tolerance] X % diet) for poultry and swine. 4. Residues in alfalfa meal are based on the tolerance in alfalfa hay, and residues in soybean meal are based on the to lerance in soy

bean seeds. Conclusions: Reassessment of the currentl y established livestock tolerances is not required for this petition. **5.3. 5**  **Food Handling (860.1460)** There are no proposed uses that are relevant to this guideline topic. **5.3. 6**  **Water, Fish and Irrigated Crops (860.1400)**  There are no proposed uses that are relevant to this guideline topic **5.4 Food Residue Profile**  Residue s of methoxyfenozide are expected to occur at moderate (up to 6.0 ppm in caneberries and sorghum grain) to high levels (up to 400 ppm in dried herbs) from the new uses proposed in the current action . **6.0 Tolerance Derivation**  In fresh herbs, subgroup 19A (except chives), the petitioner proposed a tolerance of 70 ppm, based on OECD’s tolerance calculatio n procedure. The petitioner entered all 10 individual sample residues into the MRLcalculator. When the average residues from each of the 5 basil field trials were entered, as the OECD guidance stipulates, the resulting recommended tolerance would be 80 ppm. In dried herbs, subgroup 19A (except chives), the petitioner proposed a tolerance of 400 ppm, based on OECD’s tolerance calculation procedure. However, the Agency has determined that setting separate subgroup 19A tolerances in fresh and dried commodities is not feasible from a regulatory perspective. Therefore, HED recommends setting the tolerance in the entire subgroup 19A (both fresh and dried commodities), except chives, at the higher level of 400 ppm.Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 34 of 45 In caneberries, subgroup 13 - 07A, the petitioner proposed a tolerance of 6.0 ppm, based on the OECD’s tolerance calculation procedure. HED concurs with the proposed tolerance. In dates, the petitioner proposed a tolerance of 7.0 ppm, based on 4 date fie ld trials and the OECD’s tolerance calculation procedure. However, HED determined that only 3 of the trials were trul y independent. The 4 sample residues from the 2 trials deemed to be non - independent were averaged together as one input into the MRL calculator. Also, the total application rate at one of the other trials was only half the proposed maximum seasonal use rate, a difference of >25%. Ergo, the residue values from this trial were doubled, per OECD’s preliminary guidance on proportionality

of s ample residues to application rate (ChemSAC meeting; 28 March 2012) . When the average of these residues, along with the average residues from each of the other 2 field trials were entered into the MRL calculator, the resulting recommended tolerance was 8 . 0 ppm. In sorghum commodities, the petitioner proposed tolerances of 9.0, 15 and 4.0 ppm in the forage, stover and grain, respectively , of both grain and sweet sorghum, and 9.0 ppm in sweet sorghum stalks, based on OECD’s tolerance calculation procedure . A tolerance of 80 ppm in sorghum AGF was proposed, based on the sorghum processing study. However, the total application rate at the sorghum field trials was only two thirds the proposed maximum seasonal use rate, a difference of >25%. Ergo, the resid ue values from the trials were increased by half, per OECD’s preliminary

guidance on proportionality (ChemSAC meeting; 28 March 2012) . When these values were entered into the MRLcalculator, the resulting recommended tolerances were 15, 20 and 6.0 ppm in the forage, stover and grain, respectively , of both grain and sweet sorghum, and 15 ppm in sweet sorghum stalks. Similarly , when the HAFT from the sorghum field trials (2.25 ppm) was increased b y half, and multiplied by the AGF processing factor (35X), th e resulting recommended tolerance was 120 ppm in sorghum AGF. Instead of the proposed tolerances in the various tropical tree fruits (0.6 ppm), HED recommends establishing the tolerances at 0.60 ppm, in order to avoid the situation where a field sample containing residues significantly above the tolerance (0.64 ppm, for example) would be considered non - violative. For the same reason, HED recommends that the proposed tolerance of 0.5 ppm in subgroup 6C (except blackeyed and southern peas) be revised to 0 .50 ppm. The rationales for the establishment and deletion of other tolerances associated with the current action are listed in Table 6.0, below. An International Residue Limit Status s heet is appended as Attachment 1 . Data sets and results from the OECD tolerance calculation procedure for the various commodities are appended as Attachment 2.Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 35 of 45 **TABLE 6.0**  **Tolerance Derivation**  **for Methoxyfenozide.**

**Comm odity**  **Existing Tolerance (ppm)**  **Recommended**

**Tolerance (ppm) Correct Commodity Definition**  **. Rationale**  **180.544[a][1]** Herb subgroup 19A, fresh, except chives None 400 Herb subgroup 19A, except chive . Based on submitted dried basil field trial data. Herb subgroup 19A, dried, except chives None Date None 8 .0 Based on submitted crop field trial data. Caneberry subgroup 13 - 07A None 6.0 Sorghum, grain, forage None 15 Sorghum, grain, stover None 20 Sorghum, grain, grain None 6.0 Sorghum, sweet, forage None 15 Sorghum, sweet, stover None 20 Sorghum, sweet, grain None 6.0 Sorghum, sweet, stalk None 15 Grain, aspirated grain fractions 2.0 120 Based on sorghum field trial and processing study data. Pea and bean, dried shelled, except soy bean, subgroup 6C, except pea, blackeyed, seed and pea, southern, seed None 0.5 0 To harmonize with Codex MRLs. Fruit, small, vine climbing, except fuzzy kiwifruit, subgroup 13 - 07F None 1.0 Translated from grape data. Berry, low

growing, subgroup 13 - 07G, except cranberry None 2.0 Translated from strawberry data , and raised to harmonize with Codex MRL in strawberries . Fruit, pome, group 11 - 10 None 2.0 Update of group 11 , and raised to harmonize with Codex MRL in appl es . Vegetable, fruiting, group 8 - 10 None 2.0 Update of group 8 . Sugar apple None 0.6 0 Translated from avocado data. Cherimoya None 0.6 0 Atemoya None 0.6 0 Custard apple None 0.6 0 llama None 0.6 0 Soursop None 0.6 0 Biriba None 0.6 0 Pea, blackeyed, seed 4.0 4.0 Keep as exception s to subgroup 6C . Pea, southern, seed 4.0 4.0 Coriander, leaves 30 Remove Covered under subgroup 19A tolerance. Grape 1.0 Remove Covered under subgroup 1 3 - 07F tolerance. Straw berry 1.5 Remove Covered under subgroup 13 - 07 G tolerance. Okra 2.0 Remove Covered under group 8 - 10 tolerance.Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 36 of 45 **TABLE 6.0**  **Tolerance Derivation**  **for Methoxyfenozide.**

**Comm odity**  **Existing Tolerance (ppm)**  **Recommended**

**Tolerance (ppm) Correct Commodity Definition**  **. Rationale**  Pea, dry seed 2.5 Remove C overed under subgroup 6C tolerance . Bean, dry, seed 0.24 Remove **180.544[ b**  **]** Sorghum, grain, forage 30 Remove Expired time - limited tolerances. Sorghum, grain, stover 60 Remove Sorghum, grain, grain 0.05 Remove **180.544[ d**  **][ 2**  **]** Herb and spice, group 19, except coriander, leaves 4.5 Remove Replaced by the primary crop tolerance in subgroup 19A, except chive , and rotational crop tolerances in chive and subgroup 19B . Spice subgroup 19B None 4.5 These r eplace the rotational crop tolerance in group 19, except coriander leaves . Chive None 4.5 Rapeseed subgroup 20A None 1.0 Based on existing rotational crop data , and HED’s previous recommendation . Sunflower subgroup 20B None 1.0 **Attachments** Attachment 1: International Residue Limit Status sheet . Attachment 2: OECD MRL(Tolerance) Assessment Calculations.Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 37 of 45 **Attachment 1: International Residue Limit**  **Statu s**  **. Me** **thoxyfenozide (PC Code 121027**  **) Summary of US Tolerances, and International Maxim** **um Residue Limits.**  **Residue Definitions US (40CFR §180.544)**  **Canada Codex**  **Plants:** Methoxyfenozide (3 - methoxy - 2 - methylbenzoic acid 2 - (3,5 - dimethylbenzoyl) - 2 - (1,1 - dimethylethyl)hydrazide). **Livestock:** Com

bined residues of methoxyfenozide and its glucuronide metabolite, RH - 141,518 (3 - [2 - (1,1 - dimethylethyl) - 2 - (3,5 - dimethylbenzoyl) - hydrazino]carbonyl - 2 - methylphenyl - β - D glucopyranuronic acid). **Plants/Livestock:** Methoxyfenozide (3 - methoxy - 2 - methylbenzo ic acid 2 - (3,5 - dimethylbenzoyl) - 2 - (1,1 - dimethylethyl)hydrazide). **Livestock kidney/liver:** Methoxyfenozide, and its metabolite, 3 - {[2 - (1,1 - dimethylethyl) - 2 - (3,5 - dimethylbenzoyl) - hydrazino]carbonyl} - 2 - methylphenyl - β - D glucopyranuronic acid. Methoxyfeno zide (the residue is fat - soluble, but is not classified as fat - soluble with respect to its distribution in milk).

**Comm odity**  **2 Tolerance**  **(ppm) 3**  **Comm odity**  **MRL (m g/kg)**  **Comm odity**  **MRL (m**  **g/kg)** Herb subgroup 19A, except chive 400 Fresh Chinese chive 5 Fresh chive Date 8 .0 Caneberry subgroup 13 - 07A 6.0 Sorghum, grain, forage 15 Sorghum, grain, stover 20 Sorghum, grain, grain 6.0 Sorghum, sweet, forage 15 Sorghum, sweet, stover 20 Sorghum, sweet, grain 6.0 Sorghum, sweet, stalk 15 Grain, aspirated grain fractions 120 Pea and bean, dried shelled, except soybean, subgroup 6C, except pea, blackeyed, seed and pea, southern, seed 0.5 0 Bean, dry, seed 0.5 Fruit, small, vine climbing, except fuzzy kiwifruit, subgroup 13 - 07F 1.0 Grape 1 Berry, low

growing, subgroup 13 - 07G, except cranberry 2.0 S traw berry 2 Fruit, pome, group 11 - 10 2.0 A pples, crabapples, loquats, mayhaws, oriental pears, pears, quinces 1.5 Pome fruits 2Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 38 of 45 **Me thoxyfenozide (PC Code**  **121027 )**  **Summary of US Tolerances, and International Maxim um Residue**  **Limits. Residue Definitions**  **US (40CFR §180.544) Canada**  **Codex Plants:**  Methoxyfenozide (3 - methoxy - 2 - methylbenzoic acid 2 - (3,5 - dimethylbenzoyl) - 2 - (1,1 - dimethylethyl)hydrazide). **Livestock:** Com

bined residues of methoxyfenozide and its glucuronide metabolite, RH - 141,518 (3 - [2 - (1,1 - dimethylethyl) - 2 - (3,5 - dimethylbenzoyl) - hydrazino]carbonyl - 2 - methylphenyl - β - D glucopyranuronic acid). **Plants/Livestock:** Methoxyfenozide (3 - methoxy - 2 - methylbenzo ic acid 2 - (3,5 - dimethylbenzoyl) - 2 - (1,1 - dimethylethyl)hydrazide). **Livestock kidney/liver:** Methoxyfenozide, and its metabolite, 3 - {[2 - (1,1 - dimethylethyl) - 2 - (3,5 - dimethylbenzoyl) - hydrazino]carbonyl} - 2 - methylphenyl - β - D glucopyranuronic acid. Methoxyfeno zide (the residue is fat - soluble, but is not classified as fat - soluble with respect to its distribution in milk).

**Comm odity**  **2 Tolerance**  **(ppm) 3**  **Comm odity**  **MRL (m g/kg)**  **Comm odity**  **MRL (m**  **g/kg)** Vegetable, fruiting, group 8 - 10 2.0 Peppers, tomato 2 Sugar apple 0.6 0 Cherimoya 0.6 0 Atemoya 0.6 0 Custard apple 0.6 0 llama 0.6 0 Soursop 0.6 0 Biriba 0.6 0 Pea, blackeyed, seed 4.0 Pea, southern, seed 4.0 Rapeseed subgroup 20A 1.0 Sunflower subgroup 20B 1.0 **Completed:** M. Negussie, 7 May 2013. 1. Mexico adopts US tolerances , and/or Codex MRLs , for its export purposes. 2. Includes only commodities of interest for this action. 3. Tolerance values are those recommended by HED, not those proposed by the petitioner.Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 3 9 of 45 **Attachment 2: OECD MRL (Tolerance) Assessment Calculations. Basil (Dried)**  **Residues (ppm)**  92.000 102.000 188.000 60.500 109.000 **Methoxyfenozide Dried basil**  **USA 1 lb ai/A, 1**  **- day PHI**  **Total number of data (n)** 5 **Percentage of censored data** 0% **Number of non -**  **censored data** 5 **Lowest residue** 60.500 **Highest residue** 188.000 **Median residue** 102.000 **Mean** 110.300 **Standard deviation (SD)** 47.230 **Correction factor for censoring (CF)** 1.000 **Proposed MRL estimate**

**- Highest residue**  188.000

**- Mean + 4 SD**  299.221

**- CF x 3 Mean**  330.900 **Unrounded MRL**  330.900 **Rounded MRL 400**  High uncertainty of MRL estimate. [Small dataset]Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 40 of 45 **Basil ( Fresh**  **) Residues**  **( ppm**  **)** 15.200 20.800 43.400 9.880 19.200 **Methoxyfenozide Fresh basil**  **USA 1 lb ai/A, 1**  **- day PHI**  **Total number of data (n)** 5 **Percentage of censored data** 0% **Number of non -**  **censored data** 5 **Lowest residue** 9.880 **Highest residue** 43.400 **Median residue** 19.200 **Mean** 21.696 **Standard deviation (SD)**  12.844 **Correction factor for censoring (CF)** 1.000 **Proposed MRL estimate**

**- Highest residue**  43.400

**- Mean + 4 SD**  73.074

**- CF x 3 Mean**  65.088 **Unrounded MRL** 73.074 **Rounded MRL 80**  High uncertainty of MRL estimate. [Small dataset]Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 41 of 45 **Caneberries Residues (**  **ppm )**  0.680 2.500 1.200 1.800 2.200 2.000 **Methoxyfenozide Caneberry**  **USA 0.75 lb ai/A, 3**  **- day PHI**  **Total number of data (n)**  6 **Percentage of censored data** 0% **Number of non -**  **censored data** 6 **Lowest residue** 0.680 **Highest residue** 2.500 **Median residue** 1.900 **Mean** 1.730 **Standard deviation (SD)** 0.675 **Correction factor for censoring (CF)** 1.000 **Proposed MRL estimate**

**- Highest residue**  2.500

**- Mean + 4 SD**  4.428

**- CF x 3 Mean**  5.190 **Unrounded MRL** 5.190 **Rounded MRL 6**  High uncertainty of MRL estimate. [Small dataset]Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 42 of 45 **Date s**  **Residues ( ppm**  **)** 4.000 1.600 2. 300 **Methoxyfenozide Date**  **USA 1 lb ai/A**  **Total number of data (n)** 3 **Percentage of censored data** 0% **Number of non -**  **censored data** 3 **Lowest residue** 1.600 **Highest residue** 4.000 **Median residue** 2.300 **Mean** 2.633 **Standard deviation (SD)** 1.234 **Correction factor for censoring (CF)** 1.000 **Proposed MRL estimate**

**- Highest residue**  4.000

**- Mean + 4 SD**  7.570

**- CF x 3 Mean**  7.900 **Unrounded MRL** 7.900 **Rounded MRL 8**  High uncertainty of MRL estimate. [Small dataset]Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 43 of 45 **Sorghum Forage Residues (**  **ppm )**  2.550 1.155 6.000 3.000 2.400 2.550 6.750 7.500 2.700 3.600 4.650 7.200 **Methoxyfenozide Sorghum forage**  **USA 0.5 lb ai/A, 3**  **- day PHI**  **Total number of data (n)** 12 **Percentage of censored data** 0% **Number of non -**  **censored data** 12 **Lowest residue** 1.155 **Highest residue** 7.500 **Median residue** 3.300 **Mean** 4.171 **Standard deviation (SD)** 2.171 **Correction factor for censoring (CF)** 1.000 **Proposed MRL estimate**

**- Highest residue**  7.500

**- Mean + 4 SD**  12.854

**- CF x 3 Mean**  12.514 **Unrounded MRL** 12.854 **Rounded MRL 15** Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 44 of 45 **Sorghum Grain Residues (**  **ppm )**  3.000 0.930 0.255 0.435 0.390 0.795 3.450 2.100 0.225 0.480 0.510 0.690 **Methoxyfenozide Sorghum grain**  **USA 0.5 lb ai/A, 21**  **- day PHI**  **Total number of data (n)** 12 **Percentage of censored data** 0% **Number of non -**  **censored data** 12 **Lowest residue** 0.225 **Highest residue** 3.450 **Median residue** 0.600 **Mean** 1.105 **Standard deviation (SD)** 1.111 **Correction factor for censoring (CF)** 1.000 **Proposed MRL estimate**

**- Highest residue**  3.450

**- Mean + 4 SD**  5.550

**- CF x 3 Mean**  3.315 **Unrounded MRL** 5.550 **Rounded MRL 6** Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D 40 7 7 5 8

Page 45 of 45 **Sorghum Stover Residues (**  **ppm )**  5.700 0.675 3.300 1.425 1.230 2.550 7.800 9.750 1.395 6.450 11.400 6.000 **Methoxyfenozide Sorghum stover**  **USA 0.5 lb ai/A, 21**  **- day PHI**  **Total number of data (n)**  12 **Percentage of censored data** 0% **Number of non -**  **censored data** 12 **Lowest residue** 0.675 **Highest residue** 11.400 **Median residue** 4.500 **Mean** 4.806 **Standard deviation (SD)** 3.594 **Correction factor for censoring (CF)** 1.000 **Proposed MRL estimate**

**- Highest residue**  11.400

**- Mean + 4 SD**  19.183

**- CF x 3 Mean**  14.419 **Unrounded MRL** 19.183 **Rounded MRL 20**