Methoxyfenozide Summary of Analytical Chemistry and Residue Data DP Barcode D407758

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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY

WASHINGTON, DC 20460

OFFICE OF CHEMICAL SAFETY 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 Groups; to Extend the Tolerances in Grapes and Strawberries to Their

Respective Subgroups, and in Avocadoes to Various Tropical Tree Fruits; to 

Remove the Tolerances 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 Analytical Chemistry and Residue Data. 

PC Code: 121027 DP Barcode: D407758

Decision Number: 472142 Registration Number: 62719-442

Petition: 2E8118 Regulatory Action: Section 3

Risk Assessment Type: NA Case Number: 7431

TXR Number: NA CAS Number: 161050-58-4

MRID Numbers: 48994101-04 40 CFR: §180.544

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), 7505P
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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 Analytical Method/Multiresidue Methods.......................................... 8

2.2.2 Recommended Tolerances........................................................................................ 8

2.2.3 Revisions to Petitioned-For Tolerances.................................................................... 9

2.2.4 International Harmonization ................................................................................... 10

2.3 Label Recommendations................................................................................................ 11

2.4 Submittal of Analytical Reference Standards (860.1650) ............................................. 11

3.0 Chemical Identity............................................................................................................... 12

3.1 Nomenclature................................................................................................................. 12

3.2 Physicochemical 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 Analytical 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)..................................................................... 30
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5.3.4 Meat, Milk, Poultry and Eggs (860.1480) .............................................................. 32

5.3.5. Food Handling (860.1460)...................................................................................... 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 Residue Limit Status sheet................................................37 

Attachment 2: OECD MRL (Tolerance) Assessment Calculations...................................39 
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1.0 Executive Summary

Methoxyfenozide (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 lepidopterous 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 soybean aspirated grain fractions (40CFR §180.544[a][1]). 

Permanent tolerances are also established for residues of methoxyfenozide 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-141,518) in eggs and meat byproducts at 0.02-0.40 ppm (40CFR 

§180.544[a][2]). Additionally, permanent 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 metabolites 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 expired on 31 December 2012. 

The Interregional Research Project Number 4 (IR-4) has submitted a petition requesting the 

establishment of permanent tolerances for residues of methoxyfenozide in or on dates;

caneberries (subgroup 13-07A); grain sorghum forage, stover and grain; sweet sorghum forage,

stover, grain and stalks; aspirated grain fractions (AGF), based on sorghum data; dried shelled 

peas and beans, except soybeans (subgroup 6C), except blackeyed peas and southern peas; fresh 

herbs (subgroup 19A), except chives; and dried herbs (subgroup 19A), except chives. 

Tolerances were requested in the updated crop groups 8-10 and 11-10 (from groups 8 and 11, 

respectively), and in the updated subgroups 13-07F and 13-07G (from grapes and strawberries, 

respectively). Tolerances in sugar apples, cherimoyas, atemoyas, custard apples, ilamas, 

soursops and biribas were also requested, based on translation of avocado residues. 

Additionally, rotational crop tolerances in the rapeseed subgroup (20A) and the sunflower 

subgroup (20B) were requested. The proposed new uses in dates, caneberries, sorghum and 

herbs are supported by magnitude-of-residue data generated by IR-4. Other changes are

supported by data previously reviewed by the Agency in 2009. The requested rotational crop 

tolerances in the rapeseed and sunflower subgroups are based on 2012 recommendations by

EPA. The petition proposes 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 soybeans (subgroup 6C) was proposed at the 

Agency's request to better harmonize with existing Codex MRLs. The existing tolerances in 

dried beans and dried peas would be removed concurrently with the establishment of tolerance in 

subgroup 6C. The tolerance in okra would be removed concurrently with the update of crop 

group 8 to crop group 8-10. The tolerances in grapes and strawberries would be removed 

concurrently with the establishment of the tolerances in crop subgroups 13-07F and 13-07G, 

respectively. The primary crop tolerance in coriander leaves, along with the rotational crop 
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tolerance in herbs and spices (group 19), except coriander leaves, would be removed 

concurrently with the establishment of the primary crop tolerance in subgroup 19A, except 

chives. Although not proposed in the petition, rotational crop tolerances would necessarily 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 uses, 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 flowable 

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 80 ppm in fresh herbs (subgroup 19A) except chives, and a tolerance of 400 ppm in 

dried herbs (subgroup 19A) except chives. However, HED has determined that it would be 

preferable to set a tolerance in the entire crop subgroup (herbs subgroup 19A, except chives) 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 (MI, 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 conducted 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 in 
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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 days, and 0.29-9.7 (0.45-7.6) ppm in sorghum stover harvested at a 

PHI of 21-23 days. Following 4 foliar broadcast applications of the 2 lb ai/gal FlC formulation 

to sweet sorghum (only 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 days. 

These field trial data support tolerances of 6.0 ppm in both sweet and grain sorghum grain, 

tolerances 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. 

Processing data were submitted for sorghum (sweet sorghum syrup 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 days, 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 syrup and sorghum AGF, respectively. 

These data indicate that methoxyfenozide did not concentrate in sweet sorghum syrup (1X

processing factor), but did concentrate in sorghum AGF (35X processing factor). Ergo, a 

tolerance in sweet sorghum syrup 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 methods were used for the quantitation of 

methoxyfenozide residues in samples from the various crop field trial and processing studies, 

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 uses will not result in 

revisions to the existing tolerances in livestock commodities. 

MRL Harmonization: Codex has not established maximum residue limits (MRLs) 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 MRLs in fresh Chinese chive leaves and fresh chive leaves at 5 mg/kg. 

There are no Canadian MRLs 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/MRLs in herbs and caneberries. 
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Codex has established MRLs 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 in 

the updated pome fruits 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 MRL in 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 MRL in 

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 MRLs in avocadoes or papayas. The recommended tolerance of 0.50 ppm in 

dried shelled peas and beans, except soybeans (subgroup 6C) was proposed at the Agency's 

request to better harmonize with the existing Codex MRL of 0.5 mg/kg in dried beans. This 

tolerance would replace the current tolerances of 0.24 ppm in dried beans, and 2.5 ppm in dried 

peas, which would both be removed. 

2.0 Regulatory Recommendations

HED has examined the residue chemistry database for methoxyfenozide. Pending submission of 

a revised Section F (to propose tolerance levels and additional commodities in accordance with 

those recommended by HED, and to correct the commodity definition for the herb subgroup 

19A), there are no residue chemistry issues that would preclude establishing tolerances in the 

requested commodities. The recommended tolerances are listed in Table 2.2.2, below. 

Note to RD: Analytical standards for 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 has been replenished by the registrant. Additionally, the RH117236 metabolite standard expires on 3 September 2013. The registrant should resubmit new 

analytical reference standards, or updated certificates of analysis (COAs), for all 3 of these

standards, most urgently for the expired RH-152072 and RH-141518, but also for RH-117236 

before its expiration date. See 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]). 
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Concurrent with the establishment of the tolerance in group 8-10, the tolerances 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 the tolerance in subgroup 13-07G, the tolerance in 

strawberries should be removed (40CFR §180.544[a][1]). 

Concurrent with the establishment of the tolerance in subgroup 19A (except chives), the 

tolerance in coriander leaves 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 Considerations

2.2.1 Enforcement Analytical Method/Multiresidue Methods

Adequate methods using high performance liquid chromatography with ultraviolet or mass 

spectrometric detection (HPLC/UV or /MS) are available for enforcing the current tolerances for 

methoxyfenozide in primary and rotational crops, and in animal commodities. Depending on the 

plant commodity, the limits of quantitation (LOQs) for methoxyfenozide in primary crop 

commodities are 0.01-0.05 ppm. 

Data concerning the recovery of methoxyfenozide using the FDA multiresidue method protocols 

(PAM Volume I) were previously submitted to, and reviewed by, HED. Methoxyfenozide was 

not recoverable by 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.

Commodity as Proposed by the 

Petitioner

Proposed 

Tolerance (ppm)

Recommended 

Tolerance (ppm)

Comments; Correct 

Commodity Definition

Herb subgroup 19A, fresh, except chives 70 400 Herb subgroup 19A, except 

Herb subgroup 19A, dried, except chives 400 chive

Caneberry subgroup 13-07A 6.0 6.0
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TABLE 2.2.2 Tolerance Summary for Methoxyfenozide.

Commodity 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 

OECD calculator inputs were 

increased 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 

soybean, subgroup 6C, except pea,

blackeyed, seed and pea, southern, seed

0.5 0.50 Revise tolerance from 0.5 

ppm to 0.50 ppm. 

Fruit, small, vine climbing, except fuzzy 

kiwifruit, subgroup 13-07F

1.0 1.0

Berry, low growing, subgroup 13-07G, 

except cranberry

1.5 2.0 Tolerance harmonized 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 tolerances from 0.6

Cherimoya 0.6 0.60 ppm to 0.60 ppm. 

Atemoya 0.6 0.60

Custard apple 0.6 0.60

llama 0.6 0.60

Soursop 0.6 0.60

Biriba 0.6 0.60

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. The 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 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.
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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 truly 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 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 residue 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 MRL calculator, 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 by half, and multiplied by the AGF processing factor (35X), the 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. 

2.2.4 International Harmonization

Codex has not established MRLs 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 MRLs in fresh Chinese chive leaves and fresh chive leaves at 5 

mg/kg. There are no Canadian MRLs 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/MRLs in herbs and 

caneberries. 

Codex has established MRLs 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 in 
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the updated pome fruits 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 MRL in 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 MRL in 

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 MRLs in avocadoes or papayas. The recommended tolerance of 0.50 ppm in 

dried shelled peas and beans, except soybeans (subgroup 6C) was proposed at the Agency's 

request to better harmonize with the existing Codex MRL of 0.5 mg/kg in dried beans. This 

tolerance would replace the current tolerances of 0.24 ppm in dried beans, and 2.5 ppm in dried 

peas, which would both be removed. 

2.3 Label Recommendations

None. 

2.4 Submittal of Analytical Reference Standards (860.1650)

The analytical 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 Analysis Division’s (BEAD’s) Analytical Chemistry

Branch (ACB) of 9 May 2013. 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 by the registrant. Additionally, the RH-117236 metabolite standard expires on 3 

September 2013. The registrant is required to maintain reasonable amounts of the analytical 

reference standards for methoxyfenozide and its 4 metabolites. New reference standards, or 

updated COAs, should be sent to the ACB, which is located at Fort Meade, MD. It should be 

sent to the attention of either Theresa Cole or Thuy Nguyen at the address listed below, along 

with a letter of transmittal. Please note that the full 9-digit ZIP Code is required, 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 analytical method 

used, a statement of principal impurities, purification procedures employed, storage 

requirements, and special precautions for safe handling. Replacement of standards may be 

required periodically if supplies are exhausted, if the standards expire, or if decomposition 
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occurs during storage. Material Safety Data Sheets (MSDSs) must accompany all analytical 

standards as specified by the Occupational Safety and Health Administration (OSHA) in 

29CFR§1910.1200. In addition to the parent compound, 4 metabolites (included in risk 

assessment) are currently available in the NPSR, as listed below with their respective expiration 

dates. 

Methoxyfenozide metabolite RH-117236 3 September 2013

Methoxyfenozide metabolite RH-141518 26 July 2013

Methoxyfenozide metabolite RH-151055 15 July 2014

Methoxyfenozide metabolite RH-152,072 10 October 2010

3.0 Chemical Identity

Methoxyfenozide is a diacylhydrazine insecticide used on a variety of crops for control of 

armyworms 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 currently 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 Methoxyfenozide Nomenclature.

Chemical structure

Common name Methoxyfenozide

Company experimental name RH-2485

Molecular formula C22H28N2O3

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).

CH3

O

N

H

N

O

CH3

CH3

H C3

CH3

H3C O

CH3
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3.2 Physicochemical Characteristics

TABLE 3.2 Physicochemical Properties of Methoxyfenozide.

Parameter Value Reference

Melting point/range (oC) 206.1-208 D231303, H. Podall, 19 

pH 7.0 May 1997

Density (g/cm3) 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

Methoxyfenozide is a solid under ambient conditions, and has a somewhat low volatility. The 

compound has a relatively low solubility in water, and moderate solubility in 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 (Registration #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 

Per Season

Max. Seasonal 

Use Rate

(lb ai/A)1

PHI1

(Days)

Use Directions, Application Timing, 

and Limitations

Herbs (Subgroup 19A) Except Chives

Foliar; Ground and 

Aerial

0.12 NS21.0 1 Minimum RTI3of 10 days. Ground 

application: Apply in a minimum of 10 

GPA4to 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. 
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TABLE 3.3 Summary of Directions for Use of Methoxyfenozide. 

Application Type; 

Equipment

Use Rate

(lb ai/A)

Max. Uses 

Per Season

Max. Seasonal 

Use Rate

(lb ai/A)1

PHI1

(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, 215 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 

10GPA. 

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-Treatment Interval. 

4. GPA = Gallons Per Acre. 

5. Minimum PHI of 3 days for forage and sweet sorghum stalks, and 21 days for grain and stover. 

Conclusions: The use 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 

patterns. 

4.0 Metabolite/Degradate Residue Profile

4.1 Nature of the Residue

Metabolism Assessment Review Committee (MARC) Memo; D258034 W. Wassell; 23 July 1999

D251225; W. Wassell; 27 July 1999

D259989; W. Wassell; 8 August 2000

The nature of methoxyfenozide 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 of 
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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 methoxyfenozide residues in rotational crops is adequately understood, based on 

acceptable metabolism studies in confined, 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-151,055, 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. 

Metabolism Assessment Review Committee (MARC) Memo; D258034 W. Wassell; 23 July 1999

The nature of the residue in ruminants and poultry is adequately 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 kidney) 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 byproducts 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, RH131,157 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, RH131,157 and RH-152,071

Parent methoxyfenozide and 

metabolites RH-151,055, RH152,072, and RH-117,236
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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 

Byproducts

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 

Byproducts

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)

Metabolism 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 methoxyfenozide residues in rotational crops is adequately understood, based on 

the available confined rotational crop study. Following three soil applications of 

14C-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 days 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 biomolecules, yielding bound residues and precursors in the sugar synthesis pathway. 

4.1.3 Summary of Rat Metabolism

Risk Assessment Document D388978; M. Collantes; 23 May 2012 (PP#1E7842)

In the rat, 14C-radiolabeled methoxyfenozide 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 0.50-

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 T1/2 of 0.2-0.6 hours, and a β-phase T1/2 of 15.2-35.6 hours, 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 Cmax (0.25 hr) observed in the intestinal tract, stomach, 

liver and residual carcass. Enterohepatic circulation was observed. 
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Methoxyfenozide did not show a potential for bioaccumulation. By 5 days post-treatment, the 

highest levels were observed in the liver and carcass, but tissue radioactivity in all tissues was 

insignificant by that time. Excretion of radiolabel was essentially complete by 48 hours postdosing. 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. Methoxyfenozide was extensively metabolized. The major 

routes of metabolism involved o–demethylation and oxidative hydroxylation 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-117,236, 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-demethylation and 

oxidative hydroxylation 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 dose), consistent with 

saturation of absorption. In the bile, up to 24 metabolites were detected, with the primary

metabolite (13-18% of dose) being derived by glucuronide conjugation at the o-demethylated 

alpha ring. 

4.1.4 Summary of Environmental Degradation

EFED Memo; D388876; K. Milians; 17 August 2011

Methoxyfenozide is very persistent (T1/2 = 1 to 3 years in soil and water), and moderately mobile 

(Koc = 219–922 L/kgoc in various soils). It is stable to photolysis and hydrolysis, is not 

significantly volatile, and degrades only very slowly by microbial activity. Degradates are 

predominantly RH-117,236 and RH-131,154, but these are only 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

MRIDs #48994101 to -04
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Basil: Samples of fresh and dried basil were analyzed for residues of methoxyfenozide using 

high performance liquid chromatography with tandem mass spectrometric detection 

(LC/MS/MS) according to a slight modification of Dow AgroSciences 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, 

respectively, 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 methoxyfenozide 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. 

Briefly, residues of methoxyfenozide were extracted from the homogenized samples with 

methanol/0.1N HCl (9:1, v/v). After filtration, the filtrate was brought to known volume with 

methanol/0.1N 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 dryness with rotary evaporation 

before the sample was reconstituted in water/acetonitrile (7:3, v/v) containing 0.01% formic acid 

for analysis by LC/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, respectively, in fresh basil, and 0.0163 and 0.0489 ppm, respectively, 

in dried basil. The method was adequately validated prior to, and in conjunction with, the

analysis 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

(%)

Mean ± Std. 

Dev. (%)1

Method Validation Recoveries

Fresh leaves 

and stems

0.01 6 84, 75, 93, 692, 74, 71 78 ± 9

0.30 3 88, 87, 87 87 ± 1

10.0 3 86, 86, 99 90 ± 8
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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

(%)

Mean ± 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

0.30 2 933, 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 analyzed for residues of 

methoxyfenozide via LC/MS/MS using a modification of Dow AgroSciences Method GRM: 

02.25. This method has been assessed previously, 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 expected residue levels. No residues of methoxyfenozide 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 and using vacuum filtration; substituting a PFP phase for the 

SB-C8 phase HPLC column; and adjusting the mobile phase to use ammonium acetate instead of 

formic acid. 

Briefly, residues of methoxyfenozide were extracted from the homogenized samples with 

methanol/0.1N 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/10mM

ammonium acetate (1:1, v/v) for analysis by LC/MS/MS in the positive ionization mode. 

MS/MS detection of methoxyfenozide monitored the ion transition from m/z 369→149. 

Based on recoveries of samples fortified at the LLMV (0.05 ppm), the method LOD and LOQ

were calculated to be 0.0040 and 0.012 ppm, respectively. The method was adequately validated 

prior to, and in conjunction with, the analysis of caneberry field trial samples (see Table 5.1.1.2). 
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TABLE 5.1.1.2 Summary of Method Validation and Concurrent Recoveries of Methoxyfenozide from 

Caneberries.

Matrix Spike Level (ppm) Sample Size (n) Recoveries (%) Mean ± Std. Dev. (%)1

Method Validation Recoveries

Blackberries 0.05 3 90, 91, 89 90 ± 1

0.50 3 93, 91, 91 92 ± 1

5.0 3 89, 88, 91 89 ± 2

Concurrent Recoveries

Blackberries,

raspberries2

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 samples were analyzed for residues of methoxyfenozide via LC/MS/MS using a 

procedure derived from Dow AgroSciences 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 expected residue 

levels. No residues of methoxyfenozide equal to or above the LLMVs were detected in any of 

the control samples. 

Briefly, residues of methoxyfenozide were extracted from the homogenized samples with 

methanol/0.1N 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/10mM

ammonium acetate (1:1, v:v) for analysis by LC/MS/MS in the positive ionization mode. 

MS/MS detection of methoxyfenozide monitored the ion transition from m/z 369→149. 

Based on recoveries of samples fortified at the LLMV (0.01 ppm), the method LOD and LOQ

were calculated to be 0.0040 and 0.012 ppm, respectively. The method was validated prior to,

and in conjunction with, the analysis 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 (%) Mean ± Std. Dev. (%)*

Method 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 ± 1
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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 (%) Mean ± 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 analyzed 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 methoxyfenozide equal to or above the LLMV were 

detected in any control samples. 

Briefly, residues of methoxyfenozide were extracted from the homogenized samples with 

methanol/0.1N 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/10mM

ammonium acetate (1:1, v:v) for analysis by LC/MS/MS in the positive ionization mode. 

MS/MS detection of methoxyfenozide monitored the ion transition from m/z 369→149.

The method LOD and LOQ, respectively, 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 syrup. The LLMV 

for all sorghum matrices was 0.01 ppm. The method was validated prior to, and in conjunction 

with, the analysis of sorghum field trial and processing study samples (see Table 5.1.1.4). 

TABLE 5.1.1.4 Summary of Method Validation and Concurrent Recoveries of Methoxyfenozide from 

Sorghum Commodities.

Sorghum Matrix Spike Level (ppm) Sample Size (n) Recoveries (%) Mean ± Std. Dev. (%)1

Method Validation Recoveries

Forage 0.01 3 88, 85, 1312

101  26

0.10 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

0.10 3 84, 85, 85 85  1

1.0 3 87, 86, 86 86  1

Stover 0.01 3 75, 72, 75 74  2

0.10 3 80, 77, 78 78  2

1.0 3 80, 82, 82 81  1
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TABLE 5.1.1.4 Summary of Method Validation and Concurrent Recoveries of Methoxyfenozide from 

Sorghum Commodities.

Sorghum Matrix Spike Level (ppm) Sample Size (n) Recoveries (%) Mean ± Std. Dev. (%)1

Concurrent Recoveries

Forage 0.01 3 75, 77, 78 77  2

0.10 3 83, 83 83

10 3 87, 88, 89 88  1

Stalks 0.10 1 86 86

Grain 0.01 2 88, 78 83

0.10 1 87 87

1.0 1 89 89

5.0 3 89, 88, 89 89  1

Stover 0.01 2 602, 57259

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 reviewer.

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-Residue Methods (860.1360)

D249438, D249458, D251218 & D251225; W. Wassell; 27 July 1999

Data concerning the recovery of methoxyfenozide using the FDA multiresidue method protocols 

(PAM Volume I) were previously submitted to, and reviewed by, HED. Methoxyfenozide was 

not recoverable by 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 HPLC/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 34-99-74. 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 Biological and Economic Analysis 

Division’s (BEAD’s) Analytical Chemistry Branch (ACB) concluded that PMV trials were not 

required for the other methods, since they are similar to the validated methods. 

For each of these methods, residues of methoxyfenozide 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 the 
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DCM fraction are further purified by elution through one or more of the following column types: 

basic alumina, silica gel, carbon, Florisil, or C18. Residues in the final eluate are concentrated, 

re-dissolved in ACN/water, and analyzed by reverse-phase HPLC using UV (240 nm) or MS 

(m/z 367) with external standards. The LOQ for methoxyfenozide 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 HPLC/UV method that determines methoxyfenozide residues 

in high-moisture rotational crops, and an HPLC/MS method that determines 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), 

respectively. Samples were analyzed 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 days in fresh basil and dried basil, respectively. The data 

demonstrate that residues of methoxyfenozide were stable in the fresh and dried basil samples for 

intervals of up to 760 and 758 days (25.0 and 24.9 months) of frozen storage, respectively. Zeroday 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 Duration1

(Days [Months])

Interval of Demonstrated Storage 

Stability2(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). 
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TABLE 5.2.2 Stability of Methoxyfenozide in Basil Matrices.

Basil Matrix Spike 

Level

(ppm)

Storage 

Interval1

(Days)

Fresh 

Fortification 

Recoveries (%)

Recovered 

Residues (%)

Mean 

Recovery 

(%)

Corrected 

Recovery

(%)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 reviewer. 

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 analysis, for 130-189 days 

(4.3-6.2 months). Samples were analyzed within 0-1 days of extraction. No storage stability

data were provided. Samples for a concurrent storage stability study were prepared; however, 

they were not analyzed because the protocol stated that analysis of these samples would be 

required only in the event of a freezer failure. Existing storage stability data indicate that 

methoxyfenozide is stable at ≤-20°C for intervals of up 629 days in citrus fruits (D396397; W.T. 

Drew; 2 March 2012). 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 #586722), sugar beet roots (PMRA #1843187), and 

tomatoes (PMRA #586720). These data are adequate to support the storage conditions and 

durations of the caneberry samples from the submitted field trials. 

TABLE 5.2.3 Summary of Storage Conditions.

Matrix Storage 

Temperature (°C)

Actual Storage Duration1

(Days [Months])

Interval of Demonstrated Storage 

Stability2(Days [Months])

Caneberries -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 (refer to D396397; W.T. Drew; 2 March 2012). 

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 analysis, for 104-131 days 

(3.4-4.3 months). Samples were analyzed on the day 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 5.2.5, below. Stability during frozen storage was evaluated 

after an interval of 118 days. The data demonstrate that residues of methoxyfenozide were stable 

in date samples for intervals of up to 118 days (3.9 months) of frozen storage. 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 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. 
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TABLE 5.2.4 Summary of Storage Conditions.

Date Matrix Storage Temperature

(°C)

Actual Storage Duration1

(Days [Months])

Interval of Demonstrated Storage 

Stability2(Days [Months])

Dried fruit -20 104-1313[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 

Interval1(Days

[Months])

Procedural Recoveries 

[Mean] (%)2

Recovered Residues 

(%)

Mean 

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 reviewer. 

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), respectively. Samples were analyzed 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, below. Stability during frozen storage 

was evaluated after intervals of 607, 598 and 599 days in forage, grain and stover, respectively. 

The data demonstrated that residues of methoxyfenozide were stable in the forage, grain and 

stover samples for intervals of up to 607, 598 and 599 days (19.9, 19.6 and 19.7 months), 

respectively. 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% as 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 Duration1

(Days [Months])

Interval of Demonstrated Storage 

Stability2(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.
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TABLE 5.2.7 Stability of Methoxyfenozide in Sorghum Matrices.

Sorghum 

Matrix

Spike Level

(ppm)

Storage 

Interval1

(Days)

Fresh Fortification 

Recoveries [Average2] 

(%)

Recovered 

Residues (%)

Mean 

Recovery2

(%)

Corrected 

Recovery3

(%)

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 reviewer.

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 methoxyfenozide (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 RTIs of 9-11 days, for total application rates of 0.988-1.032 lb ai/A. 

Applications were made using backpack sprayers, in spray volumes of 21-43 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 PHIs of 1, 3, 6 and 12 days 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 Table 5.3.1.1, below). As noted previously 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 values summarized below. In the residue decline trial, the per-trial
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average residues at PHIs of 1, 3, 6 and 12 days were 43.4, 14.3, 11.5 and 0.823 ppm, 

respectively, which demonstrated that residues decreased with longer PHIs. 

TABLE 5.3.1.1 Summary of Residue Data from Basil Field Trials with Methoxyfenozide.

Basil 

Commodity

Total Use 

Rate (lb ai/A)

[g ai/ha]

PHI 

(Days)

Residue Levels (ppm)

1

n Min. Max. LAFT2 HAFT2 Median Mean 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 -- -- 100 110 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) supervised 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 NIS as an adjuvant (0.01-0.13% v/v). Samples of berries were harvested at a 

PHI of 3 days at all trial sites. At one field trial, berries were harvested at PHIs 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 methoxyfenozide 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 PHIs of 1, 3, 6 and 13 days were 2.3, 2.2, 1.8 and 1.6 ppm,

respectively, which demonstrated that residues decrease with longer PHIs. 
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TABLE 5.3.1.2 Summary of Residue Data from Caneberry Field Trials with Methoxyfenozide. 

Commodity Total Use

Rate (lb ai/A)

[g ai/ha]

PHI 

(Days)

Residue Levels (ppm)

1

n Min. Max. LAFT2 HAFT2 Median Mean Std. Dev.

Caneberries 0.744-0.778

[834-872]

3 1210.62 2.5 -- -- 1.90 1.70 0.65

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. Statistics 

were calculated by the study reviewer. 

2. LAFT = Lowest Average Field Trial; HAFT = Highest Average Field Trial. 

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 approximately 10 miles of each 

other. For purposes of OCSPP Residue Chemistry Test Guideline 860.1500 data requirements, 

the Trials 10-CA22 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 RTIs of 9-11 days, for total application rates 

of 0.501-0.933 lb ai/A. Applications were made using skid pump sprayers, in spray volumes of 

64.65-291 GPA of water, using an NIS, or a combined vegetable oil concentrate and silicone 

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 

canopy, wetting the fruit bunches to runoff. All remaining applications in all trials were made 

according to this amendment. The amendment was necessitated by 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 methoxyfenozide 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. 
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TABLE 5.3.1.3 Summary of Residue Data from Date Field Trials with Methoxyfenozide.

Date 

Commodity

Total Use 

Rate (lb ai/A)

PHI 

(Days)

Residue Levels (ppm)

1

n Min. Max. LAFT2 HAFT2 Median Mean Std. Dev.

Dried fruit 0.501-0.933 7 8 1.5 3.3 1.6 2.3 2.0 2.0 0.70

1. Except for the minimum and maximum, values reflect per-trial averages; n = number of field trials; statistics were 

calculated by the study reviewer. 

2. LAFT = Lowest Average Field Trial; HAFT = Highest Average Field Trial. 

3. The number of trials equals 3 instead of 4 because trial pair 10-CA22/10-CA23 constitutes a single trial with 

replicate samples (for purposes of OCSPP 860.1500 data requirements). 

Sorghum: IR-4 submitted field trial data for methoxyfenozide 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 trials 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 type. 

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 RTIs of 9-14 days, for total 

application rates of 0.478-0.494 lb ai/A. Applications were made using ground equipment with 

CO2 or compressed air as the propellant, in spray volumes of 8-49 GPA of water, using an NIS 

or a crop oil concentrate (COC) as an adjuvant. In the grain sorghum trials, forage was harvested 

at PHIs of 2-4 days; grain was harvested at PHIs of 11 days (one trial only) or 21-23 days, and 

was allowed to dry for 0-5 days prior to collection; and stover was harvested at PHIs 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 PHIs of 0, 7, 11 and 14 days to assess residue decline. In 

the sweet sorghum trial, stalks were harvested at a PHI of 3 days. 

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 methoxyfenozide 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 days, and 0.29-9.7 (0.45-7.6) ppm in sorghum 

stover harvested at a PHI of 21-23 days (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 methoxyfenozide were 0.045-0.18 (0.11) ppm in sorghum 

stalks harvested at a PHI of 3 days. In the residue decline trial, the per-trial average residues in 
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grain sorghum forage harvested at PHIs of 0, 4, 7, 11 and 14 days 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. LAFT2 HAFT2 Median Mean 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 establishment of 

permanent tolerances 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 limited and extensive rotational crop field trials are available that 

support these rotational crop restrictions. 

Because the maximum seasonal use rate being proposed for dates and herbs (1.0 lb ai/A) is the 

same as for other registered field and vegetable crops, no changes are required in the current 

rotational crop restrictions. 

The petitioner has proposed inadvertent tolerances in oilseed crops (the rapeseed subgroup 20A, 

and the sunflower 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 methoxyfenozide 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 

RTIs of 9-11 days, for a total application rate of 0.481 lb ai/A. Applications were made using 
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ground equipment (boom sprayers), in a spray volume of 15-21 GPA of water, containing an NIS 

as an adjuvant. 

Bulk samples of the RACs, sweet sorghum stalks, and sorghum grain, were collected at PHIs of 

3 and 21 days, respectively. The RACs were processed within 56-80 days of harvest into 

sorghum AGF, and sweet sorghum syrup, using simulated commercial procedures. 

Samples of sorghum stalks and grain, and the processed sorghum commodities, were analyzed 

for residues of methoxyfenozide 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 methoxyfenozide equal to or above the LLMV were detected in any control samples. 

Samples of sorghum stalks and grain were stored frozen, from harvest to extraction, for 21.0 and 

19.4 months, respectively. Samples of sorghum AGF and syrup were stored frozen from 

collection until extraction, for 16.7 and 18.4 months, respectively. Samples were analyzed on

the day of extraction. Storage stability data generated concurrently with the study demonstrated 

that residues of methoxyfenozide were stable in sorghum forage, grain, AGF and syrup for up to 

19.9, 19.6, 17.3 and 18.4 months), respectively. 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 conditions and durations of samples from the submitted sorghum processing 

study. 

Residues of methoxyfenozide were 1.1 and 0.48 ppm in sorghum stalks and grain (RACs) 

harvested at PHIs of 3 and 21 days, respectively, following the last of 4 foliar broadcast 

applications of Intrepid 2F at a total rate of 0.481 lb ai/A. Residues of methoxyfenozide were 1.1 

and 17 ppm in sorghum syrup and sorghum AGF, respectively (see Table 5.3.3, below). These 

data indicate that methoxyfenozide did not concentrate in sweet sorghum syrup (1X processing 

factor), but did concentrate in sorghum AGF (35X 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 --

Syrup 1.1 1X

Grain (RAC) 0.481 21 0.48 --

AGF 17 35X

* PHI = Pre-Harvest Interval. 
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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 currently 

established tolerance in AGF, from 2.0 to 120 ppm. A tolerance in sweet sorghum syrup is not 

required. 

5.3.4 Meat, Milk, Poultry and Eggs (860.1480)

No livestock feeding studies were submitted with this petition. Previously, the maximum 

reasonably 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 currently established in livestock commodities. 

TABLE 5.3.4 Calculation of Maximum Reasonably Balanced Dietary Burdens of Methoxyfenozide 

Residues to Livestock. 

Feedstuff Type1 % Dry 

Matter2

% Diet2 Established 

Tolerance (ppm)

Dietary Contribution 

(ppm)3

Beef Cattle

Alfalfa hay R 89 15 150 25.28

Field corn grain CC 88 35 0.05 0.020

Soybean AGF CC 85 5 160 9.412

Sorghum grain CC 86 40 6.0 2.790

Soybean seed PC 89 5 1.00 0.056

TOTAL BURDEN -- -- 100 -- 37.6

Dairy Cattle

Grass forage R 25 25 18 18.00

Alfalfa hay R 35 20 150 33.71

Sorghum grain CC 86 45 6.0 3.135

Undelinted cotton seed PC 88 10 2.00 0.227

TOTAL BURDEN -- -- 100 -- 55.1

Poultry

Sorghum grain CC 86 75 6.0 4.500

Alfalfa meal4PC 89 5 150 7.500

Soybean meal4PC 92 20 1.00 0.200

TOTAL BURDEN -- -- 100 -- 12.2
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TABLE 5.3.4 Calculation of Maximum Reasonably Balanced Dietary Burdens of Methoxyfenozide 

Residues to Livestock. 

Feedstuff Type1 % Dry 

Matter2

% Diet2 Established 

Tolerance (ppm)

Dietary Contribution 

(ppm)3

Swine

Sorghum grain CC 86 80 6.0 4.800

Field corn grain CC 88 5 0.05 0.043

Soybean meal 4PC 92 15 1.00 0.150

TOTAL BURDEN -- -- 100 -- 4.99

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 

tolerance in soybean seeds. 

Conclusions: Reassessment of the currently 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

Residues 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 calculation procedure. The 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 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.
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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 field trials and the 

OECD’s tolerance calculation procedure. However, HED determined that only 3 of the trials 

were truly 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 (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 residue 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 MRL calculator, 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 by half, and multiplied by the AGF processing factor (35X), the 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 sheet is appended as Attachment 1. Data sets and results 

from the OECD tolerance calculation procedure for the various commodities are appended as 

Attachment 2. 
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TABLE 6.0 Tolerance Derivation for Methoxyfenozide. 

Commodity 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 

Herb subgroup 19A, dried, except basil field trial data. 

chives

None

Date None 8.0 Based on submitted crop field 

Caneberry subgroup 13-07A None 6.0 trial data. 

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 

soybean, subgroup 6C, except pea, 

blackeyed, seed and pea, southern, seed

None 0.50 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 apples. 

Vegetable, fruiting, group 8-10 None 2.0 Update of group 8. 

Sugar apple None 0.60 Translated from avocado data. 

Cherimoya None 0.60

Atemoya None 0.60

Custard apple None 0.60

llama None 0.60

Soursop None 0.60

Biriba None 0.60

Pea, blackeyed, seed 4.0 4.0 Keep as exceptions to subgroup 

Pea, southern, seed 4.0 4.0 6C. 

Coriander, leaves 30 Remove Covered under subgroup 19A

tolerance. 

Grape 1.0 Remove Covered under subgroup 13-07F

tolerance. 

Strawberry 1.5 Remove Covered under subgroup 13-07G

tolerance. 

Okra 2.0 Remove Covered under group 8-10

tolerance. 
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TABLE 6.0 Tolerance Derivation for Methoxyfenozide. 

Commodity Existing

Tolerance (ppm)

Recommended 

Tolerance (ppm)

Correct Commodity Definition.

Rationale

Pea, dry seed 2.5 Remove Covered under subgroup 6C 

Bean, dry, seed 0.24 Remove tolerance. 

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 replace 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. 
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Attachment 1: International Residue Limit Status. 

Methoxyfenozide (PC Code 121027)

Summary of US Tolerances, and International Maximum 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: Combined residues of 

methoxyfenozide and its glucuronide 

metabolite, RH-141,518 (3-[2-(1,1-

dimethylethyl)-2-(3,5-dimethylbenzoyl)-

hydrazino]carbonyl-2-methylphenyl- β-Dglucopyranuronic acid). 

Plants/Livestock: Methoxyfenozide 

(3-methoxy-2-methylbenzoic 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-Dglucopyranuronic acid. 

Methoxyfenozide (the residue 

is fat-soluble, but is not 

classified as fat-soluble with 

respect to its distribution in 

milk). 

Commodity2 Tolerance 

(ppm)3

Commodity MRL (mg/kg) Commodity MRL 

(mg/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

0.50 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 Strawberry 2

Fruit, pome, group 11-10 2.0 Apples, crabapples, 

loquats, mayhaws, 

oriental pears, pears, 

quinces

1.5 Pome fruits 2
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Methoxyfenozide (PC Code 121027)

Summary of US Tolerances, and International Maximum 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: Combined residues of 

methoxyfenozide and its glucuronide 

metabolite, RH-141,518 (3-[2-(1,1-

dimethylethyl)-2-(3,5-dimethylbenzoyl)-

hydrazino]carbonyl-2-methylphenyl- β-Dglucopyranuronic acid). 

Plants/Livestock: Methoxyfenozide 

(3-methoxy-2-methylbenzoic 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-Dglucopyranuronic acid. 

Methoxyfenozide (the residue 

is fat-soluble, but is not 

classified as fat-soluble with 

respect to its distribution in 

milk). 

Commodity2 Tolerance 

(ppm)3

Commodity MRL (mg/kg) Commodity MRL 

(mg/kg)

Vegetable, fruiting, group 8-

10

2.0 Peppers, tomato 2

Sugar apple 0.60

Cherimoya 0.60

Atemoya 0.60

Custard apple 0.60

llama 0.60

Soursop 0.60

Biriba 0.60

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. 
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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]
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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]
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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]
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Dates

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]
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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
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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
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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