UNITED STATES ENVIRONMENTAL PROTECTION AGENCY

WASHINGTON, D.C. 20460

OFFICE OF CHEMICAL SAFETY

AND POLLUTION PREVENTION

MEMORANDUM

Date: 9/7/2012

SUBJECT: Fluazinam. Petitions for the Establishment of Tolerances and Registration of 

New Uses on Soybeans, the Melon Subgroup (9-A), and the Pepper/Eggplant 

Subgroup (8-10B). Summary of Analytical Chemistry and Residue Data

PC Code: 129098 DP Barcodes: D397721, D398888, D399475

Decision Nos.: 459107, 459565, 461245 Registration Nos.: 71512-1

Petitions: 1E7959, 8E7506, 2F7977 Regulatory Action: Section 3 Registration

Risk Assessment Type: Single Chemical

Aggregate

Case No.: 7013

TXR No.: NA CAS No.: 79622-59-6

MRID Nos.: 48704501, 48704502,

 48707301, 48712601

40 CFR: §180.574

 

FROM: Douglas Dotson, Ph.D., Chemist

Risk Assessment Branch II

Health Effects Division (7509P)

THROUGH: Dennis McNeilly, Chemist

Risk Assessment Branch II

Health Effects Division (7509P)

TO: Andrew Ertman/Barbara Madden, RM Team 5, RIMUERB

Dominic Schuler/Tony Kish, PM Team 22, Fungicide Branch

Registration Division (7505P)

Executive Summary

Fluazinam (3-chloro-N-[3-chloro-2,6-dinitro-4-(trifluoromethyl)phenyl]-5-(trifluoromethyl)-2-

pyridinamine) is a member of the phenyl-pyridinamine class of compounds. It is a non-systemic, 

preventive, contact fungicide with a multi-site mode of action. When applied to plants, it 
Fluazinam Summary of Analytical Chemistry and Residue Data DP No. 397721

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remains primarily on the plant surface, it is not taken up to any extent by the plant, and it is not 

translocated within the plant. Fluazinam operates by disrupting the production of energy at 

several metabolic sites within the fungal cell.

Tolerances have been established in 40 CFR §180.574(a)(1) for residues of fluazinam in/on plant 

commodities at levels ranging from 0.01 in or on Brassica leafy vegetables (Crop Group 5) to 

7.0 ppm in or on the Bushberry subgroup (13-07B). A tolerance has been established in 40 CFR 

§180.574(a)(2) for residues of fluazinam and its metabolite AMGT on wine grapes at 3.0 ppm 

(40 CFR). Finally, a tolerance of 0.05 ppm has been established for fluazinam and its 

metabolites AMPA and DAPA and their sulfamate conjugates in or on the fat and meat 

byproducts of cattle, goats, horses, and sheep.

The registrants, ISK Biosciences and the Interregional Research Project No. 4 (IR-4) submitted

two petitions to establish tolerances for fluazinam in/on soybeans and the commodities of the 

melon and pepper/eggplant subgroups (9-A and 8-10B, respectively). In addition, the registrant 

submitted residue data for the metabolite, AMGT (see Table 2 for chemical name and structure), 

on lettuce in order to fulfill a condition of registration cited in a previous HED risk assessment. 

This document summarizes the available residue chemistry data in support of the tolerance 

petitions. The end-use product (EP) relevant to all petitions is OMEGA®500F (EPA Reg. No. 

71512-1), a flowable concentrate (FlC) formulation containing 40% fluazinam (equivalent to 

4.17 lb ai/gal). 

In PP# 2F7977, ISK Biosciences requested the registration of fluazinam for use on soybeans. In 

conjunction with this petition, the registrant proposed tolerances of 0.01 ppm for soybean seed 

and 0.02 ppm for soybean hulls. In PP# 1E7959, IR-4 requested the registration of fluazinam for 

use on the commodities of the melon and pepper/eggplant subgroups. In conjunction with this 

petition, IR-4 proposed tolerances of 0.08 ppm for melons and 1.5 ppm for peppers and eggplant. 

In a previous tolerance petition, PP#8E7506, IR-4 requested registration of fluazinam for use on 

both head and leaf lettuce. In conjunction with this use, a tolerance of 0.02 ppm was established 

for head lettuce and a tolerance of 2.0 ppm was established for leaf lettuce. HED cited the 

following data deficiency with respect to the lettuce field trials: “Samples from the lettuce field 

trial need to be analyzed for residues of AMGT. The residue data should also be supported by

data depicting the frozen storage stability of AMGT in the lettuce samples. HED recommends 

that these data be made a condition of registration” (D360840, D. Dotson, 3/31/2010). IR-4 

submitted the requested data. The data are adequate. Residues of AMGT were below the LOQ 

of 0.01 ppm in all field trial samples. 

Use Directions

The registrant submitted adequate use directions for the application of fluazinam to soybeans as 

well as the commodities of the melon and pepper/eggplant subgroups. The use directions are 

sufficient to allow for evaluation of the submitted residue data relative to the proposed use 

patterns. The available field trial data support the proposed use directions for the crops 

addressed in this summary document.
Fluazinam Summary of Analytical Chemistry and Residue Data DP No. 397721

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Nature of the Residue

The nature of fluazinam residues in plants is adequately understood based on metabolism studies 

on potatoes, peanuts, and grapes. The Agency previously concluded that the residue of concern 

in peanuts and root and tuber vegetables is parent fluazinam for purposes of both dietary risk 

assessment and tolerance enforcement. For all other crops, the residues of concern include both 

fluazinam and its metabolite AMGT for purposes of dietary risk assessment. For setting 

tolerances, the residues of concern in plants include fluazinam and AMGT for wine grapes, but 

only fluazinam for all other plant commodities.

The nature of the residue in rotational crops is adequately understood. Based on the absence of 

metabolites containing the intact fluazinam nucleus, HED has determined that the residue of 

concern in rotational crops is the parent compound, and that rotational crop tolerances are not 

required. The available confined field rotational crop study supports the 30-day plant-back 

interval (PBI) that is currently listed on the label for crops without direct uses of fluazinam.

The nature of the residue in livestock is also understood based on acceptable goat and hen 

metabolism studies. The fluazinam residues of concern in livestock commodities for tolerance 

enforcement and risk assessment were determined by HED to be parent plus the metabolites 

AMPA and DAPA, and their sulfamate conjugates.

Analytical Methods

Enforcement Method

An adequate GC/ECD method (6148-94-0170-MD-001) is available for enforcing fluazinam 

tolerances on plant commodities. The method was adequately radiovalidated and underwent a 

successful ILV trial. The method was forwarded to BEAD’s Analytical Chemistry Branch 

(ACB) for a TMV trial, and was subsequently determined to be suitable as a toleranceenforcement method. The method LOQ is 0.01 ppm for fluazinam in plant commodities. An 

adequate enforcement method for determination of AMGT is also available. The method is an 

HPLC/UV method entitled “Method Evaluation for the Analysis of AMGT in Grapes.” The 

registrant submitted an adequate ILV for the method. The range of fortification levels and the 

percent recovery values were acceptable.

Data-Collection Methods

Samples collected in the cantaloupe and pepper field trials, as well as in the soybean field trials 

and storage stability study, were analyzed for residues of fluazinam and AMGT using 

LC/MS/MS methods that were based on the GC/ECD plant enforcement method. The methods 

are adequate for data collection based on acceptable method recovery data included in the 

reviewed studies. The fortification levels used in the method validation trials bracketed the 

expected field residues. The LOQ was 0.01 ppm in all tested commodities. The LOD was 

0.0045 ppm in cantaloupes and peppers and 0.003 ppm in soybean seed, forage, and hay. In all 

trials, the data-collection method was validated prior to and in conjunction with the analysis of

the field trial samples.
Fluazinam Summary of Analytical Chemistry and Residue Data DP No. 397721

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Multiresidue Methods

Adequate FDA multiresidue method (MRM) testing data are available for fluazinam and its

metabolite AMGT. As fluazinam is partially recovered through Sections 302, 303, and 304 of 

PAM Volume I, the MRMs can serve as a confirmatory procedure for residues of fluazinam. 

The FDA MRM methods are not suitable for determining residues of AMGT.

Storage Stability

The registrant submitted storage stability data for soybeans. The data are adequate and indicate

that residues of fluazinam and AMGT are relatively stable in/on soybean forage, hay, and seed 

stored frozen for up to 153 days (5.0 months).

Field Trials

The submitted field trial data for fluazinam on soybeans, cantaloupes, and peppers are acceptable 

and support the proposed uses. Adequate numbers of trials were conducted in the appropriate 

geographic regions at ~1x the maximum proposed rate, and the appropriate samples were 

collected from each test at the proposed PHI. The data support the establishment of tolerances of 

0.01 ppm on soybean seed, 0.07 ppm for melons, and 0.09 ppm for peppers and eggplant. The 

OECD MRL calculation procedures were used for determining appropriate tolerance levels. The 

conditional AMGT residue data for lettuce and the supporting storage stability data are 

acceptable. 

Processing Studies

The submitted soybean processing study is adequate. Following application of fluazinam at a 1x 

application rate, residues of fluazinam and AMGT were each below the LOQ (<0.01 ppm) in/on 

all samples of soybean seed (RAC) and AGF; therefore, processing factors were not calculated 

for AGF. Following application of fluazinam at a 10x application rate, fluazinam residues 

concentrated in hulls (5.3x) and in refined oil (1.1x), but did not concentrate in meal (processing 

factor of <0.22x). Residues of AMGT were below the LOQ in/on seed, hulls, meal, and refined 

oil; therefore, processing factors were not calculated. The observed concentration factors were 

less than the theoretical concentration factors.

Analytical Reference Standards

Analytical reference standards for fluazinam, AMPA, DAPA, and AMGT are currently available 

in the EPA National Pesticide Standards Repository. The analytical standards for AMPA and 

DAPA are due to expire in June and July of 2017, respectively. The standard for AMGT is due 

to expire in December 2012. By that date, the registrant will need to submit a new standard or an 

updated certificate of analysis for the current AMGT standard.
Fluazinam Summary of Analytical Chemistry and Residue Data DP No. 397721

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MRL Harmonization

There are currently no Codex or Mexican maximum residue limits (MRLs) for fluazinam on 

melons, bell peppers, non-bell peppers, or soybeans.

There are no Canadian MRLs for melons or peppers. The petition for melons and peppers is 

being evaluated jointly by the U.S. and Canada’s PMRA. Both countries are using the OECD 

MRL calculation procedures to determine the recommended tolerances. For this reason, the 

MRLs for melons and peppers will be harmonized between the two countries. There is a 

Canadian MRL of 0.10 ppm for edible-podded soybean. There is no need to harmonize this 

MRL with HED’s recommended tolerance of 0.01 ppm for soybean seed because edible-podded 

soybean and soybean seed are different commodities. Edible-podded soybean is an immature 

seed that includes the pod. It is likely to have a higher residue level than soybean seed, which is

the dried seed alone.

Regulatory Recommendations and Residue Chemistry Deficiencies

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

revised Section F, there are no residue chemistry issues that would preclude granting full 

registration for the requested use of fluazinam on soybeans, the melon subgroup, and the 

pepper/eggplant subgroup. The recommended tolerances are listed in Table 1.

Table 1. Tolerance Summary for Fluazinam

Commodity as Proposed by 

Registrant

Proposed Tolerance 

(ppm)

Recommended 

Tolerance (ppm)

Comments; Correct Commodity 

Definition

Melon subgroup 9A 0.08 0.07

Pepper/eggplant subgroup 8-

10B

0.10 0.09

Soybean, Seed 0.01 0.01 Soybean, seed

Soybean, Hulls 0.02 0.05 Soybean, hulls

860.1550 Proposed Tolerances

 The registrant needs to submit a revised Section F in which the tolerances and correct 

commodity definitions recommended in Table 1 are proposed.

Background

Fluazinam is a contact, multi-site fungicide with activity against a number of plant pathogenic 

fungi. It disrupts the production of energy at several metabolic sites within the fungal cell. 

Fluazinam is a protectant fungicide that remains primarily on the plant surface. It is not taken up 

to any extent by the plant, and is not translocated within the plant. The nomenclature for

fluazinam and its metabolites AMGT, AMPA, and DAPA is presented in Table 2, and the

physicochemical properties of fluazinam are summarized in Table 3. 
Fluazinam Summary of Analytical Chemistry and Residue Data DP No. 397721

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Table 2. Fluazinam Nomenclature

Compound

Common name Fluazinam

Company experimental name IKF-1216

IUPAC name 3-chloro-N-(3-chloro-5-trifluoromethyl-2-pyridyl)-α,α,α-trifluoro-2,6-dinitro-ptoluidine

CAS name 3-chloro-N-[3-chloro-2,6-dinitro-4-(trifluoromethyl)phenyl]-5-(trifluoromethyl)-

2-pyridinamine

CAS registry number 79622-59-6

End-use product (EP) Omega®500F Fungicide (EPA Reg. No. 71512-1)

Compound

Common name AMGT

Chemical name 3-[[4-amino-3-[[3-chloro-5-(trifloromethyl)-2-pyridinyl]amino]-2-nitro-6-

(trifluoromethyl) phenyl] thio]-2-(beta-D-glucopyranosyloxy) propionic acid)

Compound

Common name AMPA

Chemical name 2-(6-amino-3-chloro- α,α,α.-trifluoro-p-toluidino)-3-chloro-5-(trifluoromethyl) 

pyridine

Cl

N

H

CF3

NO2

O2N

N

Cl

F3C

O

OH

OH

OH

HO

O

NH

CF3

O2N

N

F Cl 3C

NH2

S

HOOC

Cl

N

H

CF3

O2N

N

Cl

F3C NH2
Fluazinam Summary of Analytical Chemistry and Residue Data DP No. 397721

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Table 2. Fluazinam Nomenclature

Compound

Common name DAPA

Chemical name 3-chloro-2-(2,6-diamino-3-chloro-α,α,α.-trifluoro-p-toluidino)-5-

(trifluoromethyl)pyridine

Table 3. Physicochemical Properties of the Technical Grade Fluazinam

Parameter Value References 

Melting Point/Range 115-117oC DP# 335640, 8/22/07, 

pH 5.85 W. Drew

Density (25oC) 1.02 g/cm3

Water Solubility (25oC) 0.131 mg/L (pH buffered to 5)

0.157 mg/L (pH buffered to 7)

3.384 mg/L (pH buffered to 9)

Solvent Solubility (g/L at 20oC) acetone: 853

dichloromethane: 675

ethyl acetate: 722

ethyl ether: 231

hexane: 8

methanol: 192

octanol: 41

toluene: 451

Vapor Pressure at 25oC 1.73 x 10-7 mm Hg

2.3 x 10-5Pa

Dissociation Constant, pKa 7.22 in 50% ethanol/water (v/v, average)

Octanol/Water Partition Coefficient Log Kow = 4.03 (Kow = 10,800)

UV/visible absorption spectrum (λmax, nm) 238 at pH 5

239, 342 at pH 7

260, 343, 482 at pH>10

860.1200 Directions for Use

There is currently a single end-use product (EP) for fluazinam registered in the U.S. for use on 

several food and feed crops. This product is Omega®500F (EPA Reg. No. 71512-1), which is a 

4.17 lb/gal FlC formulation. IR-4 is proposing to add uses on soybeans, the melon subgroup 

(9A) and the pepper/eggplant subgroup (8-10B). Proposed supplemental labels were provided 

for these new uses. The proposed use directions are summarized in Table 4.

Cl

N

H

CF3

N

Cl

F3C NH2

H2N
Fluazinam Summary of Analytical Chemistry and Residue Data DP No. 397721

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Table 4. Summary of Directions for Use of Fluazinam

Applic. Timing, 

Type, and Equip. Formulation1

Applic. 

Rate 

(lb ai/A)†

Max. No. 

Applic. per 

Season

Max. Seasonal 

Applic. Rate 

(lb ai/A)

PHI 

(days)

Use Directions and 

Limitations

Melons (Crop Group 9A)

Broadcast; Ground, 

Chemigation 

(Sprinkler System).

OMEGA®500F 

40% ai, Soluble 

Concentrate 

(4.17 lb ai/gal)

0.78 lb ai/A 

(24 fl oz/A) 6

4.68 lb ai/A 

(144 fl oz/A) 30

Re-treatment Interval = 7-10

days. 

Apply when disease symptoms 

first appear.

Peppers (Crop Group 8-10B)

Broadcast; Ground, 

Chemigation 

(Sprinkler System), 

Soil Drench (at 

transplanting)..

OMEGA®500F 

40% ai, Soluble 

Concentrate 

(4.17 lb ai/gal)

0.78 lb ai/A 

(24 fl oz/A) 6

4.68 lb ai/A 

(144 fl oz/A) 30

Re-treatment Interval = 7-14

days.

Apply as a soil drench at 

transplanting. Foliar applications 

should begin 7 days after 

transplanting.

Soybean

Apply at early bloom 

to full bloom stage of 

development.

Broadcast; Aerial, 

Ground.

OMEGA®500F 

40% ai, Soluble 

Concentrate 

(4.17 lb ai/gal)

0.52 lb ai/A 

(16 fl oz/A) 2

1.04 lb ai/A 

(32 fl oz/A)

Growth 

Stage 

R33

Re-treatment Interval = 10-14 

days (at early pod formation).

For preventive treatment or low 

disease pressure use low rate.

Do not feed hay from treated 

field to livestock or allow 

livestock to graze on treated 

areas.

Do not apply after early pod 

formation.

1 EPA Reg. No. 71512-1

2 Maximum Single Application Rate (lb ai/A) = (1 pint/A)(16 fl oz/1 pint) (4.17 lb ai/gal)(1 gal/128 fl oz) = 0.52 lb ai/A.

3 Do not apply after growth stage R3, early pod formation.

The proposed (and current) product label for the 4.17 lb/gal FlC formulation specifies that 

applications are allowed through the following types of irrigation systems: center pivot, 

motorized lateral move, traveling gun, solid set or portable (wheel move, side roll, end tow, or 

hand move). The label contains the following rotational crop restrictions: all crops on the label 

may be replanted immediately after treatment. All other crops can be replanted 30 days after the 

last application.

Conclusions. The submitted use directions are sufficient to allow for evaluation of the submitted 

residue data relative to the proposed use patterns. The available field trial data support the 

proposed use directions for the crops addressed in this summary document.

860.1300 Nature of the Residue – Plants

MARC Decision Memo, DP# 272624, 4/23/01, W. Cutchin

Residue Chemistry Memo DP# 257115, 5/21/01, W. Cutchin

Residue Chemistry Memo DP# 335640, 8/22/07, W. Drew

The nature of the residue in plants is adequately understood, based on acceptable potato, peanut, 

and grape metabolism studies. The metabolism of fluazinam appears to be similar in tested 
Fluazinam Summary of Analytical Chemistry and Residue Data DP No. 397721

Page 9 of 25

crops. Fluazinam undergoes reduction of one of the nitro groups to an amine, forming AMPA. 

AMPA can then be conjugated with glutathione, with subsequent degradation of the glutathione 

moiety to cysteine. The AMPA-cysteine conjugate then undergoes transamination, reduction, 

and conjugation with glucose to form AMGT. In addition, both rings of fluazinam appear to be 

labile to ring cleavage, and they subsequently degrade into small fragments that can then be 

incorporated into a variety of natural plant components. The residues of concern in primary

crops for tolerance enforcement and risk assessment are listed in Table 5.

Table 5. Fluazinam Residues of Concern in Plants

Matrix Residues Included in 

Risk Assessment

Residues Included in

Tolerance Expression

Primary crop: grapes Parent fluazinam and AMGT Parent fluazinam and AMGT

Primary crop: peanuts, bulb 

vegetables, and root and tuber 

vegetables

Parent fluazinam Parent fluazinam

Primary crops: all others Parent fluazinam and AMGT Parent fluazinam

The registrant submitted an apple metabolism study (MRID 46991301). HED has not performed 

a formal review of the study. The results of the study indicate that parent fluazinam would be 

the residue of concern in apples for both risk assessment and tolerance enforcement. As a result, 

all residues of concern in apples are included in the current determinations. 

860.1300 Nature of the Residue - Livestock

The nature of the residue in livestock is adequately understood, based on adequate goat and hen 

metabolism studies. The metabolism of fluazinam in ruminants and poultry has been discussed 

previously (D272624, W. Cutchin, 4/23/01, D360840, D. Dotson, 3/31/2010).

860.1340 Residue Analytical Methods

Plant commodities

Enforcement Methods

Fluazinam

An adequate GC/ECD method (6148-94-0170-MD-001) entitled “Fluazinam: Method for the 

Analysis in Peanut Nutmeat” (MRID 43521016) is available for enforcing fluazinam tolerances 

on plant commodities. The method was adequately radiovalidated and underwent a successful 

independent laboratory validation (ILV) trial. The method was forwarded to BEAD’s Analytical 

Chemistry Branch (ACB) for a TMV trial, and was subsequently determined to be suitable as a 

tolerance-enforcement method (Memo, D266802, P. Golden, 6/22/2001). For this method, 

residues of fluazinam are extracted with methanol:acetic acid (100:2, v/v), filtered, diluted with 

0.2 N HCl, and partitioned into hexane. Residues are then further partitioned into 0.5 N NaOH, 

the aqueous phase is acidified, and residues are partitioned back into hexane. The resulting 

hexane fraction is concentrated, and residues are purified using a Florisil column eluted with 
Fluazinam Summary of Analytical Chemistry and Residue Data DP No. 397721

Page 10 of 25

hexane:ethyl ether (80:20, v/v). Residues are concentrated to dryness, redissolved in hexane, and 

analyzed by GC/ECD using external standards for quantitation. The method LOQ is 0.01 ppm 

for fluazinam in plant commodities.

AMGT

An adequate enforcement method for determination of AMGT, a residue of concern in wine 

grapes, is available. The method is an HPLC/UV method entitled “Method Evaluation for the 

Analysis of AMGT in Grapes.” The registrant submitted an adequate ILV for the method. The 

range of fortification levels and the percent recovery values were acceptable.

Data-collection Methods

Samples collected in the cantaloupe and pepper field trials, as well as in the soybean field trials 

and storage stability study, were analyzed for residues of fluazinam and AMGT using 

LC/MS/MS methods that were based on the GC/ECD plant enforcement method. The methods 

are adequate for data collection based on acceptable method recovery data included in the 

reviewed studies. The fortification levels used in the method validation trials bracketed the 

expected field residues. The LOQ was 0.01 ppm in all tested commodities. The LOD was 

0.0045 ppm in cantaloupes and peppers and 0.003 in soybean seed, forage, and hay. In all trials, 

the data-collection method was validated prior to and in conjunction with the analysis of the field 

trial samples. 

Soybeans

Homogenized soybean samples were blended with methanol:acetic acid (98:2, v:v) and shaken. 

The mixture was filtered, the filter cake was rinsed twice with methanol:acetic acid, and the 

resulting filtrates were combined and diluted to volume with methanol. Seed extracts were 

diluted with acetonitrile (ACN):water (80:20, v:v) for analysis by LC/MS/MS. Forage and hay

extracts were cleaned up using a Waters OASIS HLB extraction cartridge. Residues were eluted 

with ACN:water (80:20, v:v), and the eluate was analyzed by LC/MS/MS.

Cantaloupes and Peppers

Residues of fluazinam and AMGT were extracted from cantaloupes using 25 mL of 

methanol/acetic acid (98/2, v/v). Samples were shaken at room temperature for 30 minutes, 

filtered, and then cleaned up using a conditioned Evolute SPE cartridge. Residues were eluted 

from the column with 6 mL of acetonitrile/water (80/20, v/v) and analyzed by LC/MS/MS 

(negative ionization mode for fluazinam; positive ionization mode for AMGT).

Conclusions. Adequate methods for fluazinam and AMGT are available for enforcement of 

tolerances in crop matrices. Adequate methods were used for collection of data in the soybean, 

cantaloupe, and pepper field trials. In all trials, the data-collection method was validated prior to 

and in conjunction with the analysis of the field trial samples. 
Fluazinam Summary of Analytical Chemistry and Residue Data DP No. 397721

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860.1360 Multiresidue Methods

Parent Fluazinam

Data depicting the recovery of fluazinam through FDA multiresidue methods (MRM) were 

submitted and forwarded to FDA for review. The MRM testing data indicate that fluazinam is 

partially recovered through Sections 302, 303, and 304 of PAM Volume I, with its recovery

being dependent on which Florisil elution system is used. The MRMs can serve as a 

confirmatory procedure for residues of fluazinam.

 

Metabolite AMGT

Data depicting the recovery of AMGT through FDA MRMs were submitted in support of the 

apple petition. ISK Biosciences submitted multiresidue method testing data for the fluazinam 

metabolite AMGT following testing and analysis according to FDA Multiresidue Method Test 

Guidelines in PAM Vol. I (1/94). The Decision Tree for MRM Testing found in the 

Multiresidue Protocols was followed in determining the response patterns. Metabolite AMGT 

was tested through Protocols A, B, C, D, E, and F. Testing under Protocol G is not required 

because AMGT is not a substituted urea. The multiresidue methods were not found to be 

suitable for determining residues of AMGT because of poor recovery.

860.1380 Storage Stability

Soybeans: MRID 48712601

ISK Biosciences submitted the results of a storage stability study with fluazinam and AMGT in 

soybean matrices. Untreated samples of soybean forage, hay, and seed were fortified with each 

analyte separately at a fortification level of 0.10 ppm. Samples were placed in frozen storage at 

<-10oC and analyzed at storage intervals of 0, 37, 62, 125, and 153 days.

In the study, residues of fluazinam and AMGT were stable in/on soybean forage, hay, and seed

stored frozen for up to 153 days (5.0 months). Lower recoveries of fluazinam and AMGT were 

obtained in stored samples at the 37- and 62-day intervals than at the 125- and 153-day intervals. 

The petitioner assumed that this was an analytical variation because it occurred in all three 

matrices. The results of the storage stability studies are presented in Table 6.
Fluazinam Summary of Analytical Chemistry and Residue Data DP No. 397721

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TABLE 6. Stability of Residues of Fluazinam and AGMT in Soybean Following Storage at <-10C

Commodity Actual 

Spike Level 

(ppm)

Storage 

Interval

(days)

Recovered Residues

(ppm)

Mean Recovered 

Residues 

(ppm)

Mean 

Recovery

(%)

Corrected 

Recovery 

(%)1

Fluazinam

Soybean Forage 0.10 0 0.0965, 0.1025, 0.0960 0.0983 98.3 96.4

37 0.0785, 0.0860, 0.0715 0.0787 78.7 83.0

62 0.0755, 0.0760, 0.0670 0.0728 72.8 79.4

125 0.0835, 0.0860, 0.1040 0.0912 91.2 84.4

153 0.0820, 0.0870, 0.1020 0.0903 90.3 86.9

Soybean Hay 0.10 0 0.1200, 0.1185, 0.1070 0.1152 115.2 98.0

37 0.0720, 0.0855, 0.0700 0.0758 75.8 85.9

62 0.0730, 0.0680, 0.077 0.0727 72.7 65.8

125 0.0690, 0.0790, 0.0820 0.0767 76.7 76.1

153 0.0775, 0.0805, 0.0800 0.0793 79.3 77.8

Soybean Seed 0.10 0 0.0845, 0.0865, 0.0860 0.0857 85.7 102.9

37 0.0780, 0.0730, 0.0865 0.0792 79.2 70.8

62 0.0760, 0.0650, 0.0650 0.0687 68.7 70.1

125 0.0820, 0.0810, 0.0800 0.0810 81.0 81.2

153 0.0740, 0.0730, 0.0725 0.0732 73.2 75.6

AGMT

Soybean Forage 0.10 0 0.1075, 0.1195, 0.1180 0.1150 115.0 114.1

37 0.0865, 0.0870, 0.0790 0.0842 84.2 74.3

62 0.0930, 0.0860, 0.0820 0.0870 87.0 80.9

125 0.0835, 0.0805, 0.0920 0.0853 85.3 78.5

153 0.0855, 0.0875, 0.0945 0.0892 89.2 80.0

Soybean Hay 0.10 0 0.1175, 0.1160, 0.118 0.1172 117.2 126.7

37 0.0775, 0.0770, 0.0740 0.0762 76.2 69.2

62 0.0770, 0.0705, 0.0760 0.0745 74.5 71.3

125 0.0855, 0.0855, 0.0850 0.0853 85.3 85.8

153 0.0795, 0.0910, 0.0820 0.0842 84.2 79.8

Soybean Seed 0.10 0 0.1185, 0.1175, 0.1185 0.1182 118.2 124.1

37 0.0705, 0.0755, 0.0710 0.0723 72.3 66.4

62 0.0535, 0.0565, 0.0585 0.0562 56.2 53.9

125 0.0725, 0.0750, 0.0720 0.0732 73.2 69.4

153 0.0750, 0.0700, 0.0720 0.0723 72.3 77.4

1 Corrected for mean concurrent recovery

Conclusion: The storage stability data are adequate and indicate that residues of fluazinam and 

AMGT are relatively stable in/on soybean forage, hay, and seed stored frozen for up to 153 days 

(5.0 months).

860.1400 Water, Fish, and Irrigated Crops

There are no proposed uses that are relevant to this guideline topic.
Fluazinam Summary of Analytical Chemistry and Residue Data DP No. 397721

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860.1460 Food Handling

There are no proposed uses that are relevant to this guideline topic.

860.1480 Meat, Milk, Poultry, and Eggs

Livestock Dietary Burdens

The livestock feedstuffs associated with the proposed uses discussed in this summary document 

are soybean seed and hulls. The livestock feedstuffs associated with registered crops include 

peanut meal, processed potato waste, wet apple pomace, and carrot culls. Fluazinam is 

registered for use on Subgroup 6A, the Edible-podded legume vegetables subgroup. However, 

the approved label excludes the use on peas; therefore, feedstuffs derived from peas were not 

included in dietary burden calculations. The proposed soybean label includes restrictions that 

prohibit the feeding of soybean forage and hay to livestock.

The maximum reasonable dietary burdens of fluazinam to livestock were calculated for the 

previous risk assessment. A tolerance of 0.05 ppm was established for the fat and meat 

byproducts of cattle, goat, horse, and sheep. As a result of the establishment of tolerances for 

soybean seed and hulls, the dietary burden for beef cattle increases from 0.04 to 0.049 ppm, and 

the dietary burden for dairy cattle increases from 1.27 to 1.28 ppm. These small increases do not 

result in a need to increase the tolerances that are established for ruminant commodities. The 

dietary burdens for poultry and swine are the same as those calculated for the previous risk 

assessment. As a result, no tolerances are needed for poultry and swine commodities.

Conclusions. The current tolerances for livestock commodities are adequate.

860.1500 Crop Field Trials

DER References: 48712601.DER.doc (Soybeans)

48704501.DER.doc (Cantaloupe)

48704502.DER.doc (Peppers)

IR-4 and ISK Biociences Corporation submitted magnitude of the residue studies in which 

fluazinam and AMGT were measured in soybeans, cantaloupes, and both bell and non-bell 

peppers. In addition, ISK Biociences submitted magnitude of the residue studies in which 

AMGT was measured in both head and leaf lettuce. The results from these field trials are 

discussed below, and the residue data are summarized in Table 7. 

Soybeans (MRID 48712601)

ISK Biosciences Corporation submitted field trial data for fluazinam on soybeans. Sixteen field 

trials were conducted in the United States and Canada during the 2010 growing season in the 

North American Free Trade Agreement (NAFTA) Growing Zones 2 (NC and VA; 2 trials), 4 

(LA and AR; 2 trials), and 5 (IA, IL, IN, MN, MO, ND, OH, SD, WI, and ON; 12 trials). 
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Each trial consisted of one untreated plot and one treated plot. At each trial location, the treated 

plot received two foliar broadcast applications of a 4.17 lb ai/gal suspension concentrate (SC)

formulation of fluazinam (Omega®500F for the U.S. trials and AllegroTM 500F for the Canadian 

trial) at 0.49-0.64 lb ai/A/application, for a total seasonal rate of 0.99-1.17 lb ai/A. Applications 

were made at 9- to 11-day retreatment intervals, except for the SD trial, where the retreatment 

interval was 16 days. Applications were made using ground equipment in spray volumes of 

19.2-30.6 gal/A. No adjuvants were added to the spray mixtures. Samples were harvested from 

all trials at 29- to 35-day preharvest intervals (PHIs) for forage and hay and 56- to 94-day PHIs 

for seed. Hay samples were allowed to dry in the field for 1-15 days prior to collection, except at 

one Minnesota trial (06) where samples were allowed to dry in the field for 42 days prior to 

collection (no explanation provided). Additional forage and hay samples were harvested at PHIs 

of 10, 20, and 40 days (NC and OH trials), and additional seed samples were harvested at PHIs 

of 66, 76, and 95 days (NC; target PHI 87 days) and 36, 46, and 66 days (OH; target PHI 56 

days) to assess residue decline.

Samples were analyzed for residues of fluazinam and its metabolite AMGT using a high 

performance liquid chromatography method with tandem mass spectrometric detection

(LC/MS/MS) adapted from Ricerca, Inc. analytical methods. The limit of quantitation (LOQ; 

determined as the lowest level of method validation, LLMV) was 0.01 ppm for each analyte. 

The method was adequate for data collection based on acceptable method validation and 

concurrent recovery data. The fortification levels used in concurrent method recovery were 

adequate to bracket expected residue levels. Concurrent recoveries and residues in treated 

samples were not corrected for apparent residues in controls.

Samples were stored frozen (<-10°C) from collection to analysis for 57-150 days (1.9-4.9 

months) for forage and hay, and 38-108 days (1.3-3.6 months) for seed. Samples were analyzed 

within 0-32 days of extraction. Adequate storage stability data are available to support the 

storage conditions and durations of samples from the submitted field trials.

Following two foliar broadcast applications of the 4.17 lb ai/gal SC formulation of fluazinam at 

0.99-1.17 lb ai/A, residues of fluazinam in/on soybean forage, hay, and seed, respectively, 

harvested at a 29- to 35-day PHI (forage and hay) or a 56- to 94-day PHI (seed) were: 0.021-

3.725, <0.017-5.207, and <0.01 ppm. Residues of AMGT were below the LOQ (<0.01 ppm) 

in/on all samples of soybean forage, hay, and seed.

In the residue decline trials, average residues of fluazinam generally declined with increasing 

PHI in forage and hay. Residues of fluazinam in/on seed and residues of AMGT in/on forage, 

hay, and seed were below the LOQ (<0.01 ppm) in/on all samples; therefore, residue decline 

could not be assessed.

Melons (MRID 48704501)

IR-4 submitted field trial data for fluazinam on cantaloupes. A total of 11 cantaloupe field trials 

were conducted in the United States and Canada during the 2007 growing season encompassing 

Zones 2 (1 trial each in GA and MD), 5 (2 trials in ON), 5B (1 trial in QC), 6 (2 trials in TX), 9 

(1 trial in NM), and 10 (2 trials in AZ, 1 trial in CA). At each test location, fluazinam 
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(formulated as Omega 500F or Allegro 500F, a suspension), was applied to cantaloupes as 6 

foliar broadcast or directed applications at rates of 832 – 958 g a.i./ha/application (0.769 – 0.855 

lbs a.i./ha/application), with retreatment intervals of 6 – 9 days, for a total application rate of 

5.18 – 5.35 kg a.i./ha/season (4.62 – 4.77 lb a.i./ha/season). Commercially mature cantaloupes 

were harvested 28-32 days after the last applications. At Trial NM06 (Las Cruces, NM), 

cantaloupes were harvested at additional preharvest intervals (PHIs) of 6, 12, 19, and 34 days to 

assess residue decline behavior. No adjuvants were used in any of the spray mixtures. 

Cantaloupe samples were analyzed for residues of fluazinam and AMGT using a working 

method based on analytical method ISK/FLU/08002 (PMRA# 2140647) with a few 

modifications. Method ISK/FLU/08002 has been reviewed and deemed adequate for data 

gathering purposes in potatoes and grapes (PMRA# 2179742). The validated LOQ for each 

analyte is 0.01 ppm. The LOD was reported to be 0.0045 ppm. The working method was 

validated prior to sample analysis. Method validation recoveries from cantaloupe samples spiked 

with 0.01 – 1.0 ppm of fluazinam or AMGT ranged from 77 – 92% and 83 – 97%, respectively.

Method suitability was also verified concurrently during sample analysis. Concurrent recoveries 

from pepper samples spiked with 0.01 – 1.0 ppm of fluazinam or AMGT ranged from 84 – 101% 

and 79 – 102%, respectively. All recoveries for each analyte fell within the acceptable range of 

70 – 120%, indicating that the working method is adequate for the determination of residues of 

fluazinam and AMGT in/on cantaloupe samples from this study.

Treated cantaloupe samples were stored frozen (-20oC) for up to 1180 days prior to extraction. 

All samples were analyzed within 6 days of extraction. The freezer storage stability of fluazinam 

and AMGT residues in/on cantaloupes was assessed concurrently in this study, with control 

cantaloupe samples spiked with 1.03 ppm of fluazinam or 0.1 ppm of AMGT. The mean 

corrected residue recovery (corrected for concurrent recoveries from freshly spiked samples) ± 

SD of fluazinam in samples stored frozen for 1184 days was 113% ± 3% (n=3). The mean 

corrected residue recoveries (corrected for concurrent recoveries from freshly spiked samples) ± 

SD of AMGT in samples stored frozen for 1035 days and 1055 days were 99% ± 3% (n=3) and 

97% ± 6%, respectively. Although cantaloupe samples were stored frozen for 125 days longer 

than the demonstrated interval of storage stability for residues of AMGT, given that very good 

recoveries were observed after a storage period of 1105 days it is not likely that significant 

residue losses would be observed over the additional storage period. Furthermore, residues of 

AMGT were all below the LOQ of 0.01 ppm in all samples whose storage durations ranged from 

1111 to 1180 days. As such, there are no concerns with the stability of residues of fluazinam and 

AMGT during the frozen storage time period for the cantaloupe samples in this study. 

Total residues of fluazinam and AMGT in/on cantaloupes treated with a suspension formulation, 

as 6 foliar broadcast or directed applications at total rates of 4.62 – 4.77 lb a.i./ha/season and 

harvested at PHIs of 27-32 days, ranged from <0.020 - <0.087 ppm. The residue decline data 

indicate that total residues of fluazinam and AMGT in/on cantaloupes decline with increasing 

PHIs.

Peppers (MRID 48704502)

ISK Biosciences submitted field trial data for fluazinam on field peppers (bell peppers and non-
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bell peppers). Thirteen field trials were conducted in the United States and Canada during the 

2007 growing season. Nine of the trials were conducted using bell peppers and encompassed 

Zones 2 (1 trial each in NJ and NC), 3 (1 trial in FL), 5 (2 trials in ON), 5B (1 trial in QC), 6 (1 

trial in TX), and 10 (2 trials in CA). The remaining 4 trials were conducted using non-bell 

peppers and encompassed Zones 3 (1 trial in FL), 5A (1 trial in WI), 6 (1 trial in TX), and 9 (1 

trial in NM).

At each test location, fluazinam (formulated as Omega 500F or Allegro 500F, a suspension), was 

applied to field peppers as 6 applications (2 soil directed applications around the base of the plant 

+ 4 foliar applications) at rates of 0.412 – 0.859 lbs a.i./ha/application, with retreatment intervals 

(RTIs) of 6 – 53 days, for a total application rate of 3.99 – 4.86 lb a.i./ha/season. Commercially 

mature peppers were harvested 28 – 31 days after the last applications. At Trial 07-NJ16 

(Bridgeton, NJ), bell peppers were harvested at additional preharvest intervals (PHIs) of 7, 13, 

20, and 35 days to assess residue decline behavior. No adjuvants were used in any of the spray

mixtures.

Pepper samples were analyzed for residues of fluazinam and AMGT using a working method 

based on analytical method ISK/FLU/08002 (PMRA# 2140647) with a few modifications. 

Method ISK/FLU/08002 has been reviewed and deemed adequate for data gathering purposes in 

potatoes and grapes (PMRA# 2179742). The validated LOQ for each analyte is 0.01 ppm. The 

LOD was reported to be 0.0045 ppm. The working method was validated prior to sample 

analysis by spiking control samples with 0.01 – 1.0 ppm of fluazinam or AMGT. Method 

suitability was also verified concurrently during sample analysis at the same spiking levels for 

each analyte. All recoveries for each analyte fell within the acceptable range of 70 – 120%, 

indicating that the working method is adequate for the determination of residues of fluazinam 

and AMGT in/on pepper samples from this study.

Treated pepper samples were stored frozen (-20oC) for up to 1249 days prior to extraction. All 

samples were analyzed the same day of extraction. The freezer storage stability of fluazinam and 

AMGT residues in/on peppers was assessed concurrently in this study, with bell pepper samples 

being spiked with 1.03 ppm of fluazinam or 0.1 ppm of AMGT. The mean corrected residue 

recovery (corrected for concurrent recoveries from freshly spiked samples) ± SD of fluazinam in 

samples stored frozen for 1241 days was 93 ± 8% (n=3). The mean corrected residue recovery

(corrected for concurrent recoveries from freshly spiked samples) ± SD of AMGT in samples 

stored frozen for 1106 days was 80 ± 3% (n=3). Although pepper samples were stored frozen for 

143 days longer than the demonstrated interval of storage stability for residues of AMGT, given 

that good recoveries were observed after a storage period of 1106 days it is not likely that 

significant residue losses would be observed over the additional storage period. Furthermore, 

residues of AMGT were all below the LOQ of 0.01 ppm in all samples whose storage durations 

ranged from 1165 to 1249 days. As such, there are no concerns with the stability of residues of 

fluazinam and AMGT during the frozen storage time period for the pepper samples in this study. 

Total residues of fluazinam and AMGT in/on bell peppers and non-bell peppers treated with a 

suspension formulation, as two soil directed applications plus 4 foliar applications at a total rates 

of 3.99 – 4.86 lb a.i./ha/season and harvested at PHIs of 28 – 31 days, ranged from <0.020 -

<0.048 ppm for bell peppers and from <0.020 – 0.064 for non-bell peppers. The residue decline 
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data indicate that total residues of fluazinam and AMGT decline in/on peppers with increasing 

PHIs.

Lettuce: Head and Leaf (MRID 48707301)

ISK Biosciences previously submitted the results of 14 field trials on head and leaf lettuce

(D360840, D. Dotson, 3/31/2010). These samples were analyzed for parent fluazinam, but not 

for the metabolite AMGT (a residue of concern for risk assessment). HED made the following 

statement in its original review of the lettuce field trial data: “Samples from the lettuce field trial 

need to be analyzed for residues of AMGT. The residue data should also be supported by data 

depicting the frozen storage stability of AMGT in the lettuce samples.” This stipulation was 

necessary because the field trial samples would have been stored for a significant period of time 

between sampling and analysis. IR-4 analyzed the stored samples for AMGT and performed a 

storage stability study.

Seven of the lettuce trials were performed on head lettuce and 7 were performed on leaf lettuce. 

The trials were conducted in the U.S. during the 2005 growing season. One of the head lettuce 

trials was conducted in EPA Growing Zone 2 (MD), one was conducted in Zone 3 (FL), and 5 

were conducted in Zone 10 (4 in CA and 1 in NM). One of the head lettuce trials was conducted 

in EPA Growing Zone 2 (GA), one was conducted in Zone 3 (FL), and 5 were conducted in Zone 

10 (4 in CA and 1 in NM).

For these trials, fluazinam (4.17 lb/gal FlC) was applied to head and leaf lettuce as a single 

broadcast foliar application during vegetative development at a rate of 0.952-1.05 lb ai/A (1x the 

proposed maximum seasonal rate). Applications were made using ground equipment in volumes 

of 32-77 gal/A, and no adjuvants were used. Single control and duplicate treated samples of 

lettuce leaves or heads, with wrapper leaves attached, were harvested at commercial maturity, 

46-52 days after application for head lettuce and 20-32 days after application for leaf lettuce. 

The lettuce samples were analyzed for AMGT residues using the method “Method Evaluation 

for the Analysis of AMGT in Grapes,” Document Number 6268-94-1231-MD-001. Minor 

modifications to the analytical procedure were made to improve method performance. 

Homogenized samples were blended with acetonitrile/water (4:1, v/v). After filtration, the 

sample together with the filter paper was extracted for a second time by shaking with 

acetonitrile/water (1:1, v/v). The combined filtrate was rotary evaporated to remove all 

acetonitrile. The final extract was adjusted with acetonitrile/water (35.2:67.5, v/v) for 

LC/MS/MS analysis. The method was validated at 3 fortification levels (0.02, 0.1, and 1.0 ppm) 

prior to sample analysis. Both fortified and unfortified control samples were analyzed 

concurrently with each sample set to demonstrate the absence of significant interferences and 

adequate recoveries. The lowest level of method validation was 0.02 ppm.

In all 28 samples analyzed for AMGT, the residue level was below the LLMV of 0.02 ppm. For 

the storage stability study, the performing laboratory analyzed samples that had been stored for 

1088 to 1110 days (3.0 to 3.04 years). This storage interval was equivalent to 50-63% of the 

actual sample storage duration (4.8 to 5.9 years). IR-4 reported that additional data will be 

collected and analyzed under a separate protocol. Samples were fortified at 0.1 ppm and stored 
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in the same freezer as the field trial samples. AMGT storage stability ranged from 71-78% (n=7) 

for samples analyzed at 1088 to 1110 days. Concurrent recoveries for spikes analyzed along 

with the storage stability samples were in the range of 82-87%. HED considers the submitted 

storage stability data to be adequate to demonstrate that residues of AMGT are sufficiently stable 

in lettuce to resolve the data deficiency cited in the lettuce tolerance petition. 

Conclusions. The submitted field trial data for fluazinam on soybeans, cantaloupes, and peppers 

are acceptable and support the proposed uses. Adequate numbers of trials were conducted in the 

appropriate geographic regions at approximately 1x the maximum proposed rate, and the 

appropriate samples were collected from each test at, or close to, the proposed PHI. The 

conditional AMGT residue data for lettuce and the supporting storage stability data are also 

acceptable. 

TABLE 7. Summary of Fluazinam Field Trial Residue Data

Commodity Analyte Total

Rate

(lb ai/A)

PHI 

(days)

Residue Levels (ppm)

n Sample 

Min.

Sample 

Max.

LAFT1 HAFT2 Median Mean Std. 

Dev.

Soybeans

Soybean Forage Fluazinam 0.99-1.17 29-35 16 0.021 3.73 0.034 3.06 0.427 0.63 0.74

AMGT <0.01 <0.01 <0.01 <0.01 0.01 0.01 NA

Soybean Hay Fluazinam 29-35 16 <0.017 5.21 0.028 5.21 0.868 1.41 1.48

AMGT <0.01 <0.01 <0.01 <0.01 0.01 0.01 NA

Soybean Seed Fluazinam 56-94 16 <0.01 <0.01 <0.01 <0.01 0.01 0.01 NA

AMGT <0.01 <0.01 <0.01 <0.01 0.01 0.01 NA

Cantaloupes

Cantaloupe Fluazinam 5.18-5.35 27-32 22 <0.01 0.077 <0.01 0.048 0.01 0.017 0.015

AMGT <0.01 <0.01 <0.01 <0.01 0.01 0.01 NA

Peppers (Bell and Non-Bell)

Bell Pepper Fluazinam 4.47-5.45 28-31 18 <0.01 0.038 <0.01 0.030 0.01 0.014 0.007

AMGT <0.01 <0.01 <0.01 <0.01 0.01 0.01 NA

Non-Bell 

Pepper

Fluazinam 5.10-5.29 28-31 8 <0.01 0.053 <0.01 0.045 0.01 0.02 0.016

AMGT <0.01 <0.01 <0.01 <0.01 0.01 0.01 NA

Lettuce

Head Lettuce AMGT 0.95-1.02 46-52 14 <0.02 <0.02 <0.02 <0.02 0.02 0.02 NA

Leaf Lettuce AMGT 0.97-1.05 20-32 14 <0.02 <0.02 <0.02 <0.02 0.02 0.02 NA

1

 LAFT = lowest average field trial

2

 HAFT = highest average field trial result.

NA = not applicable

860.1520 Processed Food and Feed

Soybeans (MRID 48712601)

ISK Biosciences Corporation submitted a processing study for fluazinam on soybean. In one 

crop field trial conducted in Louisiana, soybeans grown in separate plots received two foliar 

broadcast applications of a 4.17 lb ai/gal suspension concentrate (SC) formulation of fluazinam 
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(Omega® 500F). Applications were made at a rate of 0.52-0.53 lb ai/A/application for a total 

seasonal rate of 1.05 lb ai/A to produce seed for generation of aspirated grain fractions (AGF), 

and at an exaggerated rate (10x field rate) of 5.30-5.34 lb ai/A/application for a total seasonal 

rate of 10.64 lb ai/A to produce seed for generation of processed fractions. Applications were 

made at an 11-day retreatment interval (RTI) using ground equipment in spray volumes of 19.2-

23.6 gal/A. Adjuvants were not used at either plot. Soybean seed was harvested from the plots 

at a 90-day preharvest interval (PHI) and processed into AGF, hulls, meal, and refined oil using 

simulated commercial procedures. Processing was conducted by GLP Technologies (Navasota, 

TX). The registrant provided adequate descriptions of the processing procedures, including 

material balance summaries.

Samples were analyzed for residues of fluazinam and its metabolite AMGT using a high 

performance liquid chromatography method with tandem mass spectrometric detection

(LC/MS/MS) adapted from Ricerca, Inc. analytical methods. The limit of quantitation (LOQ; 

determined as the lowest level of method validation, LLMV) was 0.01 ppm for each analyte. 

The method was adequate for data collection based on acceptable method validation and 

concurrent recovery data. The fortification levels used in method validation and concurrent 

method recovery were adequate to bracket expected residue levels (within an order of magnitude 

for hulls). Concurrent recoveries and residues in treated samples were not corrected for residues 

in controls.

Samples were stored under ambient conditions (field sites) and frozen (≤12°C at the processing 

facility and <-10°C at the analytical laboratory) from harvest/processing to analysis. Processing 

took place within 71 days of harvest. Sample analyses were completed within 77-117 days (2.5-

3.8 months) for seed (RAC) and 46 days (1.5 months) for the processed commodities. All 

samples were analyzed within 1-9 days of extraction. Adequate storage stability data are 

available to support the storage conditions and durations of samples from the submitted 

processing study.

Following application of fluazinam at 1.05 lb ai/A, residues of fluazinam and AMGT were each 

below the LOQ (<0.01 ppm) in/on all samples of soybean seed (RAC) and AGF; therefore, 

processing factors were not calculated for AGF. Following application of fluazinam at 10.64 lb 

ai/A, average residues of fluazinam were 0.044 ppm in/on seed, 0.231 ppm in hulls, 0.046 ppm 

in refined oil, and below the LOQ (<0.01 ppm) in meal. Residues of fluazinam concentrated in 

hulls (5.3x) and refined oil (1.1x), but did not concentrate in meal (processing factor of <0.22x). 

Residues of AMGT were below the LOQ in/on seed, hulls, meal, and refined oil; therefore, 

processing factors were not calculated.

The processing factors calculated in this study were less than the maximum theoretical 

concentration factors for soybean of 11.3x for hulls, 2.2x for meal, and 12.0x for oil (based on 

separation into components; OPPTS 860.1520, Table 3).
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TABLE 8. Residue Data from Soybean Processing Study with Fluazinam.

RAC Processed 

Commodity

Total 

Rate

(lb ai/A)

PHI Residues (ppm)1[Average] Processing Factor2

Fluazinam AMGT Fluazinam AMGT

Soybean Seed (RAC)31.05 90 ND, ND [<0.01] ND, ND [<0.01] -- --

AGF <0.01, <0.01 [<0.01] ND, ND [<0.01] NC4 NC

Seed (RAC)310.64 90 0.043, 0.044 [0.044] ND, ND [<0.01] -- --

Hulls 0.242, 0.220 [0.231] ND, ND [<0.01] 5.3x NC

Meal <0.01, <0.01 [<0.01] ND, ND [<0.01] <0.22x NC

Refined oil 0.047, 0.044 [0.046] ND, ND [<0.01] 1.1x NC

1

 The LOQ was 0.01 ppm for all analytes in all matrices. Per trial average residues were calculated by the study reviewer using 

the LOQ for all residues reported as <LOQ.

2

 Processing Factor = [Measured residue for analyte in the processed fraction] / [Measured residue for analyte in the seed RAC].

3

 Values for bulk seed samples shipped to the processor.

4

 NC = Not calculated; residues were below the LOQ in both the RAC and the processed fraction.

Conclusions: The submitted soybean processing study is acceptable. Following application of 

fluazinam at 1.05 lb ai/A, residues of fluazinam and AMGT were each below the LOQ (<0.01 

ppm) in/on all samples of soybean seed (RAC) and AGF; therefore, processing factors were not 

calculated for AGF. Following application of fluazinam at 10.64 lb ai/A, average residues of 

fluazinam were 0.044 ppm in/on seed, 0.231 ppm in hulls, 0.046 ppm in refined oil, and below 

the LOQ (<0.01 ppm) in meal. The processing data indicate that residues of fluazinam may

concentrate in hulls (5.3x) and may concentrate slightly in refined oil (1.1x), but do not 

concentrate in meal (processing factor of <0.22x). The observed concentration factors were less 

than the theoretical concentration factors. Residues of AMGT were below the LOQ in/on seed, 

hulls, meal, and refined oil; therefore, processing factors were not calculated. 

An acceptable method was used for residue quantitation, and the study is supported by adequate

storage stability data.

860.1650 Submittal of Analytical Reference Standards

Analytical reference standards for fluazinam, AMPA, DAPA, and AMGT are currently available 

in the EPA National Pesticide Standards Repository (electronic communication, T. Cole to D. 

Dotson, 7/18/2012). The analytical standards for AMPA and DAPA are due to expire in June 

and July of 2017, respectively. The standard for AMGT is due to expire in December 2012. The 

registrant will need to submit new standards or updated certificates of analysis for the current 

standards by their respective expiration dates.

The standards should be sent to the Analytical Chemistry Lab, which is located at Fort Meade, to 

the attention of Theresa Cole at the following address:

USEPA

National Pesticide Standards Repository/Analytical Chemistry Branch/OPP

701 Mapes Road

Fort George G. Meade, MD 20755-5350

The mail will be returned if the extended zip code is not used.
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860.1850/1900 Confined and Field Accumulation in Rotational Crops

HED previously reviewed an adequate confined rotational crop study (D360840, D. Dotson, 

3/31/2010). Based on the absence of metabolites containing the intact fluazinam nucleus, HED 

concluded that the residue of concern in rotational crops is the parent compound, and that 

rotational crop tolerances are not required for fluazinam. The 30-day PBI on the label is 

sufficient for all rotated crops not on the label. No additional rotational crop data are required 

for the proposed uses on soybeans, melons, or peppers.

860.1550 Proposed Tolerances

The residue of concern for tolerance enforcement is parent fluazinam for all plant commodities, 

except for wine grapes, for which the parent compound and the metabolite AMGT are the 

residues of concern. For poultry and ruminants, the residues of concern for tolerance 

enforcement are the parent compound plus the metabolites AMPA and DAPA, and their 

sulfamate conjugates.

Adequate numbers of field trials at ~1x the proposed use rate are available for cantaloupe, bell 

peppers, non-bell peppers, and soybeans to support the establishment of tolerances on these 

crops. Tolerances do not need to be recommended for soybean forage and hay because the label 

contains a restriction that prohibits the feeding of forage and hay to livestock.

The OECD MRL calculation procedures were used to determine the recommended tolerances, 

which are listed in Table 9. OECD MRL calculation procedures were not used for soybean seed 

because all of the residue values were below the LOQ of 0.01 ppm. HED is recommending in 

favor of a tolerance of 0.01 ppm for soybean seed.

There are currently no Codex or Mexican maximum residue limits (MRLs) for fluazinam on 

melons, bell peppers, non-bell peppers, or soybeans.

There are no Canadian MRLs for melons or peppers. The petition for melons and peppers is 

being evaluated jointly by the U.S. and Canada’s PMRA. Both countries are using the OECD 

MRL calculation procedures to determine the recommended tolerances. For this reason, the 

MRLs for melons and peppers will be harmonized between the two countries. There is a 

Canadian MRL of 0.10 ppm for edible-podded soybean. There is no need to harmonize this 

MRL with HED’s recommended tolerance of 0.01 ppm for soybean seed because edible-podded 

soybean and soybean seed are different commodities. Edible-podded soybean is an immature 

seed that includes the pod. It is likely to have a higher residue level than soybean seed, which is 

the dried seed alone.

An International Residue Limit Status Sheet can be found in Attachment 1.
Fluazinam Summary of Analytical Chemistry and Residue Data DP No. 397721

Page 22 of 25

References

D272624, Fluazinam. Decision by Metabolism Assessment Review Committee (MARC), W. 

Cutchin, 4/23/01

D360840, Fluazinam. Petitions for the Establishment of Tolerances and Registration of New 

Uses on Apples, Carrots, Lettuce, and Bulb Onion Subgroup (3-07A), and a Request for a 

Reduced Tolerance on Bushberry Subgroup (13-07B). Summary of Analytical Chemistry and 

Residue Data, D. Dotson, 3/31/2010

D387187, Fluazinam. Human Health Risk Assessment for the Section 3 Registration Action on 

Turfgrass, D. Dotson, et al., 2/7/2012

Attachments:

 

Attachment 1: International Residue Limit Status sheet

Attachment 2: Tolerance Assessment Calculations
Fluazinam Summary of Analytical Chemistry and Residue Data DP No. 397721

Page 23 of 25

Attachment 1: International Residue Limits

Fluazinam (129098; 7-10-2012)

Summary of US and International Tolerances and Maximum Residue Limits 

Residue Definition: 

US Canada Mexico2 Codex3

40 CFR 180.574:

Plants: Fluazinam, 3-chloro-N-[3-chloro2,6-dinitro-4-(trifluoromethyl)phenyl]-5-

(trifluoromethyl)-2-pyridinamine

Commodity1 Tolerance (ppm) /Maximum Residue Limit (mg/kg)

US Canada Mexico2 Codex3

Soybean, Seed 0.01 0.10 ppm: Ediblepodded soybean

Soybean, Hulls 0.02

Melon subgroup 9A 0.07

Pepper/Eggplant

Subgroup 8-10B 0.09

Completed: M. Negussie; 07/16/2012

1

Includes only commodities of interest for this action. Tolerance values should be the HED recommendations and 

not those proposed by the applicant.

2 Mexico adopts US tolerances and/or Codex MRLs for its export purposes.

3 * = absent at the limit of quantitation; Po = postharvest treatment, such as treatment of stored grains. PoP = 

processed postharvest treated commodity, such as processing of treated stored wheat. (fat) = to be measured on the 

fat portion of the sample. MRLs indicated as proposed have not been finalized by the CCPR and the CAC.
Fluazinam Summary of Analytical Chemistry and Residue Data DP No. 397721

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Attachment 2: Tolerance Assessment Calculations

Soybeans

HED’s current policy is to use OECD MRL calculation procedures to determine recommended 

tolerances. In the case of soybeans, all of the residue values were below the LOQ of 0.01 ppm. 

When all residue values are below the LOQ, HED recommends in favor of establishing the 

tolerance at the LOQ. Therefore, HED recommends in favor of a tolerance of 0.01 ppm for 

soybean seed.

The average processing factor for soybean hulls is 5.25x. Multiplying this value by the soybean 

seed LOQ of 0.01 ppm yields a value of 0.0525 ppm. HED recommends in favor of a tolerance 

of 0.05 ppm for soybean hulls.

Melon Subgroup (9A)

For melons, the OECD MRL Calculator was used for calculating recommended tolerances. 

Average cantaloupe field trial values were entered into the calculator. The dataset used to 

establish tolerances on the melon subgroup consisted of field trial data representing applications 

at rates of 4.6-4.8 lb ai/A (six applications at approximately 0.78 lb ai/A/application) with a 27-

32 day PHI. Using the MRL calculator, the recommended tolerance is 0.07 ppm. 

Pepper/Eggplant Subgroup (8-10B)

For peppers, the OECD MRL Calculator was used for calculating recommended tolerances. 

Average field trial values were entered into the calculator. Field trial data for bell and non-bell 

peppers were entered separately and the higher of the two recommended tolerances (i.e., that for 

the non-bell peppers) is the one that HED is recommending as the tolerance for the entire 

subgroup. The dataset used to establish tolerances on the pepper/eggplant subgroup consisted of 

field trial data representing applications at rates of 4.6-4.7 lb ai/A (six applications at 

approximately 0.78 lb ai/A/application) with a 28-31 day PHI. Using the MRL calculator, the 

recommended tolerance is 0.09 ppm. The MRL calculator recommends a tolerance of 0.05 ppm 

for the bell peppers. As stated above, the recommended tolerance for the non-bell peppers is 

being recommended as the tolerance for the entire subgroup because it is the higher of the two 

values. 
Fluazinam Summary of Analytical Chemistry and Residue Data DP No. 397721

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Fluazinam: OECD MRL Calculator Results

OECD MRL Calculator Results for the Melon Subgroup (9A) and the Pepper/Eggplant Subgroup (8-10B)

Compound Fluazinam Fluazinam Fluazinam

Crop Bell Peppers Non-Bell Peppers Cantaloupes

Region / Country US & Canada US & Canada US & Canada

GAP 4.47-5.45 kg a.i./ha

(3.99 - 4.86 lb a.i./A)

PHI = 28 - 31 days

5.10 - 5.29 kg a.i./ha

(4.55 - 4.72 lb a.i./A)

PHI = 28 - 31 days)

5.18 - 5.35 kg a.i./ha

(4.62 - 4.77 lb a.i./A)

PHI = 27 - 32 days

Total number of 

data points (n)

9 4 11

Percentage of 

censored data

33% 50% 45%

Number of noncensored data

6 2 6

Lowest residue 0.010 0.010 0.010

Highest residue 0.030 0.045 0.048

Median residue 0.011 0.013 0.011

Mean 0.014 0.020 0.017

Standard deviation 

(SD)

0.007 0.017 0.012

Correction factor 

for censoring (CF)

0.778 0.667 0.697

- Highest residue 0.030 0.045 0.048

- Mean + 4 SD 0.041 0.087 0.063

- CF x 3 Mean 0.034 0.041 0.036

Unrounded MRL 0.041 0.087 0.063

Rounded MRL 0.05 0.09 0.07

High uncertainty of MRL 

estimate due to small dataset.

Residues (mg/kg) Residues (mg/kg) Residues (mg/kg)

0.010 * 0.016 0.020

0.019 0.010 * 0.010 *

0.010 * 0.045 0.011

0.010 * 0.010 * 0.010 *

0.015 0.010 *

0.015 0.048

0.030 0.010 *

0.011 0.024

0.010 0.014

0.021

0.010 *