Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY

WASHINGTON, D.C. 20460

OFFICE OF PREVENTION, PESTICIDE

AND TOXIC SUBSTANCES

MEMORANDUM

Date: 3/31/2010

SUBJECT: 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.

PC Code: 129098 DP Barcodes: D360840 and D366506

Decision Nos.: 404254 and 412727 Registration No.: 71512-1

Petitions: 8E7506, 9E7570, and 9F7571 Regulatory Action: Section 3 Registration

Risk Assessment Type: NA Case No.: NA

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

MRID Nos.: 47631001, 47631002, and

 47756601 through 47756611

40 CFR: §180.574

 

FROM: Douglas Dotson, Ph.D., Chemist

Risk Assessment Branch II

Health Effects Division (7509P)

THROUGH: William Drew, Chemist

Richard Loranger, Ph.D., Senior Scientist

Risk Assessment Branch II

Health Effects Division (7509P)

TO: Laura Nollen/Barbara Madden, RM Team 5, RIMUERB

John Bazuin/Tony Kish, PM Team 22, Fungicide Branch

Registration Division (7505P)
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

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This document was originally prepared under contract by Dynamac Corporation (1901 Research 

Boulevard, Suite 220; Rockville, MD 20850 and 1910 Sedwick Rd., Building 100, Suite B; 

Durham, NC 27713). The document has been reviewed by the Health Effects Division (HED) 

and revised to reflect current Office of Pesticide Programs (OPP) policies.

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. Fluazinam is a nonsystemic, preventive, contact fungicide with a multi-site mode of action. It disrupts the 

production of energy at several metabolic sites within the fungal cell. Fluazinam is a protectant 

fungicide. That is, when applied to plants, it 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.

The Agency has received three separate tolerance petitions to establish permanent tolerances for 

fluazinam residues of concern in/on various raw agricultural and animal commodities. This 

document summarizes the available residue chemistry data in support of these 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#8E7506, the Interregional Research Project No. 4 (IR-4), on behalf of the Agricultural 

Experiment Stations of Arizona, California, Colorado, Georgia, Idaho, New York, Ohio, 

Tennessee, and Texas has requested registration of fluazinam for use on lettuce (head and leaf) 

and Onion, bulb, subgroup 3-07A. The proposed use of OMEGA®500F on lettuce is for a single 

broadcast or banded foliar application or soil drench application at crop thinning at up to 1.0 lb 

ai/A. The proposed use for the bulb onion subgroup is for a maximum of six broadcast foliar 

applications during vegetative development at up to 0.52 lb ai/A/application for a maximum 

seasonal rate of 3.1 lb ai/A. The minimum retreatment interval (RTI) is 7 days for onions, and 

both uses only allow for applications using ground equipment. The minimum preharvest 

intervals (PHIs) are 50 days for head lettuce, 30 days for leaf lettuce, and 7 days for onions. In

conjunction with these uses, IR-4 has proposed the establishment of permanent tolerances for 

residues of fluazinam in/on the following commodities:

Lettuce, head ..................................................................... 0.02 ppm

Lettuce, leaf ............................................................................ 2 ppm

Onion, bulb, subgroup 3-07A ........................................... 0.15 ppm

Also included in PP# 8E7506 is a request by IR-4 to revise the established 7.0-ppm tolerance for 

fluazinam residues in/on the Bushberry subgroup (13B) and other bushberry type crops (aronia 

berry, buffalo currant, Chilean guava, European barberry, highbush cranberry, edible 

honeysuckle, jostaberry, juneberry, lingonberry, native currant, salal, and sea buckthorn). These 

tolerances were originally established under PP# 6E7137 (Memo, D335640, W. Drew, 8/22/07). 

IR-4 is requesting that a single tolerance be established for the updated Bushberry subgroup
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(13-07B) for residues of fluazinam at a level of 4.5 ppm. This proposed tolerance would then 

replace the multiple tolerances on the various bushberries.

In PP# 9E7570, IR-4, on behalf of the Agricultural Experiment Stations of California, Georgia, 

Texas, and Washington, has requested the registration of fluazinam for use on carrots. The 

proposed use includes a maximum of four directed band applications prior to or during disease 

development at up to 0.52 lb ai/A/application, with a 7-day RTI, for a maximum seasonal rate of 

2.1 lb ai/A. Applications may be made using ground equipment. A 7-day PHI is proposed. 

Concurrently, IR-4 has proposed the establishment of the following permanent tolerance for 

residues of fluazinam:

Carrot, roots ......................................................................... 0.8 ppm

In PP# 9F7571, ISK Biosciences Corporation requested the registration of fluazinam for use on 

apples. The proposed use includes a maximum of ten broadcast foliar applications prior to or 

during disease development at up to 0.45 lb ai/A/application, with a 7-day RTI, for a maximum 

seasonal rate of 4.50 lb ai/A. Applications may be made using ground and aerial equipment. A 

28-day PHI is proposed. In conjunction with this use, ISK Biosciences has proposed the 

establishment of permanent tolerances for residues of the fungicide fluazinam and its metabolite 

AMGT in or on the following commodities:

Apples.................................................................................. 1.7 ppm

Apple, pomace, wet.............................................................. 5.0 ppm

In addition, ISK Biosciences has proposed tolerances for residues of fluazinam and its 

metabolites DAPA and AMPA in the following livestock commodities: 

Cattle, fat............................................................................ 0.03 ppm

Cattle, kidney ..................................................................... 0.03 ppm

Cattle, liver......................................................................... 0.03 ppm

Cattle, meat ........................................................................ 0.03 ppm

Cattle, meat byproducts...................................................... 0.03 ppm

Goat, fat.............................................................................. 0.03 ppm

Goat, kidney....................................................................... 0.03 ppm

Goat, liver .......................................................................... 0.03 ppm

Goat, meat.......................................................................... 0.03 ppm

Goat, meat byproducts ....................................................... 0.03 ppm

Horse, fat............................................................................ 0.03 ppm

Horse, kidney ..................................................................... 0.03 ppm

Horse, liver......................................................................... 0.03 ppm

Horse, meat ........................................................................ 0.03 ppm

Horse, meat byproducts...................................................... 0.03 ppm

Milk.................................................................................... 0.03 ppm

Sheep, fat............................................................................ 0.03 ppm

Sheep, kidney..................................................................... 0.03 ppm
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Sheep, liver ........................................................................ 0.03 ppm

Sheep, meat........................................................................ 0.03 ppm

Sheep, meat byproducts ..................................................... 0.03 ppm

Permanent tolerances have been established for residues of fluazinam in/on plant commodities at 

levels ranging from 0.01 to 7.0 ppm [40 CFR §180.574(a)(1)], and a tolerance has also been 

established for residues of fluazinam and its metabolite AMGT on wine grapes at 3.0 ppm (40 

CFR §180.574(a)(2)). No tolerances have been established for livestock commodities.

There are currently no established Codex, Canadian, or Mexican maximum residue limits 

(MRLs) for fluazinam on apples, carrots, lettuce, onions, or berry crops. Therefore, there are no 

harmonization issues for the requested tolerances.

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 fluazinam per se 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 fluazinam residues 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 for fluazinam. 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 regulatory interest in animal commodities were 

determined by HED to be parent plus the metabolites AMPA and DAPA, and their sulfamate 

conjugates.

An adequate gas chromatography with electron capture detection (GC/ECD) method (6148-94-

0170-MD-001) is available for determination of fluazinam residues in crop matrices. The 

method was deemed to be suitable for tolerance enforcement after it successfully completed the 

routes required for an enforcement method including radiovalidation, independent laboratory

validation (ILV), and tolerance method validation (TMV). Samples collected from the 

magnitude of the residue and storage stability studies were analyzed for residues of fluazinam 

using various GC/ECD methods based on, and revised slightly from, the plant enforcement 

method. The GC/ECD methods are adequate for data collection based on acceptable method 

recovery data. The lowest limit of method validation (LLMV) was 0.01 ppm in all tested 

commodities except in carrots where the LLMV was 0.02 ppm.
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An enforcement method for determination of AMGT, a residue of concern in wine grapes, is 

available. The registrant requested that the blueberry submission serve as the ILV for the 

method. The range of fortification levels and the percent recovery values are acceptable. As a 

result, HED considers the AMGT analytical portion of the blueberry field trial study to be 

adequate, and that it can serve as the ILV for the analytical method for AMGT residues in plant 

commodities.

PTRL Method 1676W was the data-collection method used for the analysis of samples collected 

from the dairy cattle feeding study. The method is written for LC/MS/MS analysis of fluazinam, 

AMPA, and DAPA in bovine milk and tissues, and for GC/MS analysis of DAPA in milk only. 

The limit of quantitation was 0.01 ppm for each analyte in milk, muscle, fat, liver and kidney. 

Preliminary method validation data showed that Method 1676W adequately recovered residues 

of fluazinam, AMPA, and DAPA in milk, muscle, and fat. However, poor and/or marginal 

recoveries were obtained for AMPA and DAPA residues in kidney and liver. Method 1676W 

was marginally validated by an independent laboratory during the third trial and following slight 

modifications to make the method more rugged. For the purpose of developing an animal 

enforcement method, radiovalidation data are required to determine whether the method can 

detect aged residues. HED forwarded Method 1676W to ACB/BEAD for a tolerance method 

validation (TMV) because the method encountered difficulties in the ILV (e.g., three attempts for 

successful validation and/or marginal recoveries with wide variability and high coefficient of 

variation). The method was forwarded to ACB/BEAD for method validation. ACB/BEAD 

reported that the lab that performed the ILV made major modifications to the original method. 

As a result, HED requested that the registrant submit a revised method that incorporated the 

revisions made by the ILV lab. ISK Biosciences revised the method and re-submitted it. 

ACB/BEAD performed a cursory review of the revised method. The registrant incorporated the 

modifications made by the ILV lab. However, the revision eliminated the cleanup steps that were

in the original method, and the only recovery data for the revised method were data provided by

the ILV lab. ACB/BEAD was concerned that the elimination of the cleanup steps could lead to 

dirty samples which would, in turn, lead to analytical problems, such as interference. 

ACB/BEAD performed no further validation of the method. As the revised method contains 

major revisions to the original method, and ACB/BEAD believes it is very likely that the revised 

method still is not adequate for sample analysis or tolerance enforcement, HED recommends that 

the registrant submit an ILV of the revised method.

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. Multiresidue method 

testing data are required for the regulated metabolites, AMPA and DAPA, in animals.

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

EPA National Pesticide Standards Repository; however an analytical standard for the AMGT 

metabolite is not currently available.
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Adequate storage stability data are available to support the storage conditions and durations of 

samples collected from the magnitude of the residue studies on apples, carrots, lettuce, and 

onions. As residues of fluazinam were found to be stable in tested crop matrices, storage 

stability corrections do not need to be applied to the recommended tolerances for fluazinam 

residues in/on apples, carrots, lettuce, and onions. Storage stability data for the fluazinam 

metabolite AMGT in apple commodities were also submitted, and showed that residues in wet 

apple pomace were reasonably stable for 12 months, but declined to an average corrected 

recovery of 58-63% at the 19-month interval, 61% at the 32-month interval, and 33% at the 37-

month interval. The submitted storage stability data for bovine milk, meat, and meat byproducts 

showed mixed results.

Based on the poor recoveries of metabolites AMPA and DAPA from liver and kidney and the 

mixed storage stability results, the residue data from the cattle feeding study are not adequate to 

satisfy data requirements. The feeding study data (adjusted for residue decline) along with the 

calculated dietary burdens for beef cattle (0.04 ppm) and dairy cattle (1.27 ppm) indicate that 

tolerances are needed for the combined residues of fluazinam and its metabolites DAPA and 

AMPA in the fat and meat byproducts of cattle and other ruminants at 0.05 ppm to support the 

proposed uses on apples and carrots and the established tolerances on potatoes and peanuts. 

However, no tolerances are required for milk and meat of ruminants, as the expected combined 

residues in these matrices are below the combined method limit of quantitation (LOQ) of 0.03 

ppm for the regulated compounds. Based on the transfer coefficients for livestock tissues and the 

relatively low dietary burden for swine of 0.003 ppm for fluazinam, tolerances for hog

commodities are not needed. A poultry feeding study is not required at this time because of the 

low dietary burden for poultry (0.005 ppm).

With the exception of the use of adjuvants, the submitted field trial data for fluazinam on head 

lettuce, leaf lettuce, bulb onions, carrots, and apples are acceptable and support the proposed 

uses. Adequate numbers of trials were conducted in the appropriate geographic regions at ~1x 

the maximum proposed rate using a representative FlC formulation, and the appropriate samples 

were collected from each test at the proposed PHI. However, no residue data were provided on 

AMGT residues in lettuce. Although AMGT residue data on lettuce are still required for 

purposes of dietary risk assessment, the available data would support tolerances of 0.02 ppm for 

head lettuce, 2.0 ppm for leaf lettuce, 0.20 ppm for the bulb onion (subgroup 3-07A), 1.5 ppm for 

apple, and 0.7 ppm for carrot. The tolerance spreadsheet (Guidance for Setting Pesticide 

Tolerances Based on Field Trial Data SOP) was used for determining appropriate tolerance 

levels.

For dietary risk assessment, HED will calculate AMGT residues in lettuce using a ratio of 0.35:1 

for AMGT:fluazinam residues (ChemSAC Memo, meeting of 2/6/08). The samples from the 

lettuce field trials still need to be analyzed for residues of AMGT. AMGT is not a residue of 

concern for risk assessment for carrots or onions; therefore, for these commodities it does not 

need to be included in the dietary exposure assessment. AMGT residues were measured in 

apples and the combined residues of parent and AMGT need to be included in the dietary

exposure assessment.
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After reevaluating the available residue data for blueberries, HED concludes that the residue data 

for fluazinam from the blueberry field trials are distributed lognormally. As a result, the 

recommended tolerance for the revised Bushberry subgroup 13-07B is 7.0 ppm, which is 

equivalent to the current tolerance for Subgroup 13B.

The apple processing study is not adequate to satisfy data requirements. In apples, the metabolite 

AMGT is a residue of concern for risk assessment. In the processing study there were no 

quantifiable residues of AMGT in raw apples. In several of the field trials that were performed, 

however, raw apples contained AMGT residues at, or above, the limit of quantitation. In a few 

cases, residues of AMGT were comparable to those of the parent fluazinam. Canadian and U.S. 

residue chemistry guidelines both stipulate that in the processing study, if residues in the raw 

agricultural commodity (RAC) are below the LOQ, but quantifiable residues occurred in the 

RAC in field trials performed at the maximum requested label rate, that the processing study

should be conducted at exaggerated rates in order to ensure that quantifiable residues will be 

present in the RAC. Quantifiable residues are needed in the RAC in order to determine a reliable 

concentration factor. As a result, the processing study needs to be repeated at a sufficiently high 

rate that residues of both parent and AMGT are quantifiable in the RAC. In the event that the 

potential for phytotoxicity exists, the application rate does not need to be greater than the rate at 

which phytotoxicity occurs.

Regulatory Recommendations and Residue Chemistry Deficiencies

No major deficiencies were noted in the current petitions that would preclude establishing 

permanent tolerances for fluazinam residues of concern on head lettuce; leaf lettuce; Onion, bulb, 

subgroup 3-07A; and Bushberry, subgroup 13-07B. In addition, the deficiency listed below for 

lettuce field trials needs to be resolved as a condition of registration. A revised Section F is 

needed as detailed below (860.1550).

Because of major data deficiencies, HED does not recommend in favor of the establishment of 

tolerances for apples or carrots. HED also does not recommend in favor of tolerances for animal 

commodities. The data deficiencies associated with the apple and carrot petitions are discussed 

below.

For PP# 8E7506, pending submission of residue data for AMGT on lettuce as a condition of 

registration, the submitted data support the proposed uses of OMEGA®500F on lettuce and 

Onion, bulb, subgroup 3-07A along with the establishment of tolerances for residues of 

fluazinam in/on:

Lettuce, head ..................................................................... 0.02 ppm

Lettuce, leaf ......................................................................... 2.0 ppm

Onion, bulb, subgroup 3-07A ........................................... 0.20 ppm

The petition also supports revising the existing Bushberry subgroup 13-B tolerance to a 

Bushberry subgroup 13-07B tolerance at 7.0 ppm along with deletion of existing individual 

tolerances on various berries as detailed in Table 13.
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List of Deficiencies

860.1200 Directions for Use

• The use directions for all the subject crops (lettuce, onions, bushberries, apples, 

and carrots) should include a prohibition against addition of adjuvants to the spray

mixture.

The following deficiency applies to both existing and proposed uses of fluazinam

860.1650 Submittal of Analytical Reference Standards

• An analytical reference standard for the AMGT metabolite is not available. RD 

should request that the registrant submit this standard to the EPA’s National 

Pesticide Repository as soon as possible.

List of Deficiencies by Petition 

PP# 8E7506 (Lettuce, Onion, Bushberry Subgroup)

860.1500 Crop 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.

860.1550 Proposed Tolerances

• The registrant should submit a revised section F in which a tolerance of 0.2 ppm is 

proposed for Onion, bulb, subgroup 3-07A, and a tolerance of 7.0 ppm is 

proposed for Bushberry, subgroup 13-07B.

PP#s 9F7570 (Carrots) and 9F7571 (Apples)

860.1340 Residue Analytical Methods

• At the present time, an analytical method is not available for enforcement of 

fluazinam tolerances in animal commodities. The registrant should submit an ILV 

of the revised method. This method needs to be adequate for analysis of parent 

fluazinam as well as the metabolites AMPA and DAPA in animal commodities 

for which tolerances will be established.
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• If the registrant resolves the data deficiencies associated with the apple and carrot 

petitions and re-submits the tolerance petitions, multiresidue method testing data 

will be required for the regulated metabolites, AMPA and DAPA, in animals.

860.1480 Meat, Milk, Poultry, and Eggs

• The residue data from the cattle feeding study are not adequate to satisfy data 

requirements. To support tolerances for apples and carrots, the registrant needs to 

submit a new cattle feeding study in which a method with better recoveries of 

AMPA and DAPA from liver and kidney was used. When this study is repeated, 

the samples need to be analyzed as soon as possible after sacrifice in order to 

minimize degradation of residues.

860.1520 Processed Food and Feed (Applies Only to Apple Petition, 9F7571)

• The apple processing study is not adequate to satisfy data requirements. The 

processing study needs to be repeated at a sufficiently high rate that residues of 

both parent and AMGT are quantifiable in the RAC. In the event that the 

potential for phytotoxicity exists, the application rate does not need to be greater 

than the rate at which phytotoxicity occurs.

Note to RD:

HED recommends that 40CFR §180.574(a)(1) be amended by replacing the tolerance expression 

with the following: “Tolerances are established for residues of fluazinam (3-chloro-N-[3-chloro2,6-dinitro-4-(trifluoromethyl)phenyl]-5-(trifluoromethyl)-2-pyridinamine), including its 

metabolites and degradates, in or on the commodities in the table below. Compliance with the 

tolerance levels specified below is to be determined by measuring only fluazinam.” HED further 

recommends that 40CFR §180.610(a)(2) be amended by replacing the tolerance expression with 

the following: “Tolerances are established for residues of fluazinam, including its metabolites 

and degradates, in or on the commodities in the table below. Compliance with the tolerance 

levels specified below is to be determined by measuring only fluazinam and its metabolite 

AMGT (3-[[4-amino-3-[[3-chloro-5-(trifluoromethyl)-2-pyridinyl]amino]-2-nitro-6-

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

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 1, and the

physicochemical properties of fluazinam are summarized in Table 2. 
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Table 1. Fluazinam Nomenclature.

Compound

Cl

N

H

CF3

NO2

O2N

N

Cl

F3C

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) 4.17 lb/gal FlC (Omega® 500F Fungicide; EPA Reg. No. 71512-1)

Compound

O

OH

OH

OH

HO

O

NH

CF3

O2N

N

F Cl 3C

NH2

S

HOOC

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

Cl

N

H

CF3

O2N

N

Cl

F3C NH2

Common name AMPA

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

pyridine
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Table 1. Fluazinam Nomenclature.

Compound

Cl

N

H

CF3

N

Cl

F3C NH2

H2N

Common name DAPA

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

(trifluoromethyl)pyridine

Table 2. 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) (pH buffered to 5) 0.131 mg/L

(pH buffered to 7) 0.157 mg/L

(pH buffered to 9) 3.384 mg/L

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 (Pa) 2.3 x 10-5at 25oC

1.3 x 10-4at 35oC

6.7 x 10-5at 45oC

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

Octanol/water partition coefficient, Log 

(KOW)

1.08 x 104(Log Kow = 4.03)

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 to ISK Biosciences in 

the U.S. for use on food/feed crops. This EP is Omega®500F (EPA Reg. No. 71512-1), which is 

a 4.17 lb/gal FlC formulation. It is registered for use on ginseng, peanuts, potatoes, turnip 

greens, Crop Group 5 (Brassica leafy vegetables), Subgroup 6A (except pea), Subgroup 6B 

(except pea), Subgroup 6C (except pea), the Bushberry Subgroup (13B), and other bushberries. 
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IR-4 is proposing to add uses on carrot, lettuce, and members of the Bulb onion subgroup, 3-

07A, to the label for the 4.17 lb/gal FlC formulation for control of fungal diseases. Proposed 

supplemental labels were provided for these new uses. The proposed use directions are 

summarized in Table 3.

ISK Biosciences is proposing to add use on apple to the product label for the 4.17 lb/gal FlC 

formulation. The proposed use directions are summarized in Table 3.

Table 3. Summary of Directions for Use of Fluazinam.

Applic. Timing; Type;

and Equipment

Formulation

[EPA Reg. 

No.]

Applic. 

Rate 

(lb ai/A)

Max. No. 

Applic. per 

Season

Max. 

Seasonal 

Applic. Rate

(lb ai/A)

PHI

(days)

Use Directions and 

Limitations1

Apple

Broadcast foliar 

applications prior to 

or during disease

development;

Ground and aerial

equipment 

4.17 lb/gal 

FlC

[71512-1]

0.33-

0.45 10 4.50 28

Apply in a minimum 

of 5 gal/A (both 

ground and aerial 

equipment). The 

minimum RTI is 7 

days.

Bulb Onion Subgroup 3-07A

Broadcast foliar 

applications prior to 

or during disease

development;

Ground equipment 

4.17 lb/gal 

FlC

[71512-1]

0.52 6 3.12 7

Apply in a minimum 

of 5 gal/A. The 

minimum RTI is 7 

days.

Carrot

Directed band to the 

crop prior to or 

during disease

development;

Ground equipment 

4.17 lb/gal 

FlC

[71512-1]

0.52 4

2.08

(implied) 7

Apply in a minimum 

of 30 gal/A. The 

minimum RTI is 7 

days.

Lettuce (Head and Leaf)

Broadcast or banded 

foliar application or 

soil drench 

application at 

thinning;

Ground equipment

4.17 lb/gal

FlC

[71512-1]

0.52-

0.99 1 1.0

50 - head 

lettuce;

30 - leaf 

lettuce

Apply in a minimum 

of 50 gal/A. 

1

 A 48-hour restricted entry interval is specified. 

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

applications are allowed through the following types of irrigations 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.
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 13 of 54

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, with the exception of 

the use of adjuvants. As the crop field trials did not include adjuvants, the use directions for all 

proposed crops should include a prohibition against the addition of adjuvants to the spray

mixture.

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 

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 regulatory interest in 

primary crops are listed in Table 4.

Table 4. 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 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); however, HED has not 

reviewed it. In the event that the registrant resolves the data deficiencies associated with the 

apple petition and re-submits it, the apple metabolism study should be reviewed.

860.1300 Nature of the Residue - Livestock

MARC Decision Memo, D272624, W. Cutchin, 4/23/01

Residue Chemistry Memo D257115, W. Cutchin, 5/21/01

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

metabolism studies. The metabolism of [14C]-fluazinam in ruminants and poultry is similar, and 

involves reduction of one or both nitro groups on the phenyl ring to form AMPA, MAPA, or 

DAPA. Fluazinam also undergoes dehalogenation and hydroxylation of the chlorine on the 

phenyl ring to form HYPA. These compounds can then undergo conjugation with glutathione, 

and subsequent degradation of the glutathione moiety yields a variety of polar compounds. 

Although the ring structure of the parent molecule remains intact, fluazinam per se was only a 
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 14 of 54

minor component (≤2.7% TRR) of the [14C]-residues in poultry tissues and eggs, and was not 

detected in ruminant tissues or milk. The residues of concern in livestock are listed in Table 5.

Table 5. Fluazinam Residues of Concern in Livestock

Matrix Residues Included in 

Risk Assessment

Residues Included in

Tolerance Expression

Ruminant Parent fluazinam, AMPA, and 

DAPA, and their sulfamate 

conjugates

Parent fluazinam, AMPA, and 

DAPA, and their sulfamate 

conjugates

Poultry Parent fluazinam, AMPA, and 

DAPA, and their sulfamate 

conjugates

Parent fluazinam, AMPA, and 

DAPA, and their sulfamate 

conjugates

860.1340 Residue Analytical Methods

Residue Chemistry Memo D335640, W. Drew, 8/22/07

Residue Chemistry Memo D212612, G. Herndon, 9/5/95

TMV Results Memo, D266802, P. Golden, 6/22/01

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 

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 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 enforcement method for determination of AMGT, a residue of concern in wine grapes, is 

available. HED recommended in a previous memorandum (Memo, D335640, W. Drew, 8/22/07) 

that a previously submitted HPLC/UV method based on Method Evaluation for the Analysis of 

AMGT in Grapes (MRID 45593101) undergo an ILV trial, and potentially, a TMV trial by the 

ACB. This method was used to measure AMGT residues in the blueberry field trials that the 
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 15 of 54

registrant performed. The method procedure and fortification recoveries were discussed in the 

DER for MRID 46986701.

 

Concurrent recoveries were measured in samples fortified with AMGT at 0.020 ppm, 0.100 ppm, 

0.200 ppm, and 1.00 ppm (1x, 5x, 10x, and 50x the LLMV). Individual recoveries of AMGT (n 

= 35) ranged from 58 to 125% (see TABLE 6, below). At each fortification level, average 

recoveries were within the generally recognized acceptable range (70-120%) except for 2 

samples spiked with 0.020 ppm AMGT (125 and 65% recovery) and 3 samples spiked with 

0.100 ppm AMGT (58, 68, and 68% recovery). Overall, peaks were well-defined and 

symmetrical in all chromatograms. Three untreated control samples showed identifiable peaks at 

or near the retention time for AMGT (ranging from 0.0333 to 0.1307 ppm). Treated sample 

chromatograms showed analyte peaks within the area of analytical interest, and no carryover 

from controls. Calibration curves were not provided for AMGT. Treated and control blueberry

samples were stored frozen (at -21 ± 7°C) for durations of up to 229 days before AMGT analysis. 

A concurrent freezer storage stability study was conducted in/on blueberry samples fortified with 

AMGT at 0.15 ppm. Residues in the concurrent freezer storage stability samples remained stable 

for intervals of 251 days. Therefore, there are no concerns with the stability of residues over time 

in this study.

TABLE 6. Summary of Method Validation and Concurrent Recoveries of AMGT from Blueberries.

Crop 

[Matrix]

Recovery 

Type 1

Spike Level

(ppm)

Sample 

Size (n)

Recoveries

(%)

Mean ± Std. 

Dev. (%)

AMGT

Blueberry 

[Berry]

MV 0.020 3 110, 95, 100 102 ± 8

MV 0.100 3 95, 81, 94 90 ± 8

MV 1.00 3 110, 110, 110 110 ± 0

CR 0.020 5 1252, 65, 70, 70, 110 88 ± 28

CR 0.100 27 93, 76, 81, 82, 71, 58, 84, 82, 78, 79, 74, 72, 

1003, 733, 70, 88, 683, 683, 1103, 703, 80, 90, 

89, 83, 84, 82, 88

80 ± 11

CR 1.00 1 77 77

CR 0.200 2 95, 80 88 ± 11

1. MV = Method Validation; CR = Concurrent Recovery.

2. High recovery might be due to a slight interference in the peak.

3. After interference found in the untreated sample is subtracted.

The registrant requested that the blueberry submission serve as the ILV for the method. The 

range of fortification levels and the percent recovery values are acceptable. As a result, HED 

considers the AMGT analytical portion of the blueberry field trial study to be adequate, and that 

it can serve as the ILV for the analytical method for AMGT residues in plant commodities. 
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 16 of 54

Data-collection Methods

Fluazinam

Samples collected from the magnitude of the residue and storage stability studies were analyzed 

for residues of fluazinam using GC/ECD methods revised from the plant enforcement method. 

The GC/ECD 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 LLMV was 0.01 ppm in all tested commodities,

except in carrots, where the LLMV was 0.02 ppm.

AMGT

Samples of apples and apple processed commodities were also analyzed for residues of AMGT 

using an HPLC/UV method similar to that reviewed in Memo, D335640, W. Drew, 8/22/2007. 

The HPLC/UV method is adequate for data collection based on acceptable method verification 

and concurrent method recoveries. The validated method LOQ was 0.01 ppm in all apple 

matrices.

Animal commodities

DER Reference: 47756602.der.doc (Includes method validation data from MRID 47756605)

ISK Biosciences submitted PTRL Method 1676W (MRID 47756602) entitled “Fluazinam, 

AMPA and DAPA Method in Milk and Tissues as Described in ‘Magnitude of Fluazinam 

Residues in Bovine Tissues and Milk from a 28-Day Feeding Study.’” Method 1676W was the 

data-collection method used for the analysis of samples collected from a companion cattle 

feeding study (MRID 47756605). As a result of a June 30, 2007 meeting between HED and ISK 

representatives to discuss concerns about the analytical approach for the feeding study, the 

method has incorporated a mild acid hydrolysis step to convert the sulfamate conjugates to free 

AMPA and DAPA. The method is written for LC/MS/MS analysis of fluazinam, AMPA, and 

DAPA in bovine milk and tissues, and for GC/MS analysis of DAPA in milk only. The reported 

method LOQ was 0.01 ppm for each analyte in milk, muscle, fat, liver, and kidney. The method 

is described briefly below.

For milk, a sample was mixed with HCl, and residues were extracted with methanol. The extract 

was concentrated, and residues were mixed with water and sodium chloride for partitioning with 

dichloromethane (DCM) or hexane for LC/MS/MS analysis for fluazinam, AMPA, and DAPA 

residues, or for GC/MS analysis of DAPA residues. For muscle, residues were extracted with 

acetonitrile (ACN)/water, with acetic acid for fluazinam and without acetic acid for AMPA and 

DAPA. After concentration and/or dilution, the extracts were cleaned up through a solid phase 

extraction (SPE) column prior to LC/MS/MS analysis. For fat, residues were extracted with 

ACN/water with acetic acid, then again with ACN. The combined extract was diluted for 

partitioning with ACN-saturated cyclohexane. The ACN phase was evaporated and reconstituted 

for LC/MS/MS analysis. For analysis of liver and kidney using the non-hydrolysis method, 
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 17 of 54

residues were extracted with ACN/water with acetic acid, then again with ACN/water. The 

combined extract was diluted, concentrated, and mixed in water with sodium chloride for 

partitioning with DCM prior to LC/MS/MS analysis. For analysis of liver and kidney using the 

hydrolysis method, residues were extracted with ACN/water. The extract was diluted and 

concentrated prior to the addition of HCl (held for 1 hour at 37°C). Water and sodium chloride 

were added for partitioning with hexane (liver) or ethyl acetate (kidney). The hexane phase was 

concentrated and reconstituted for LC/MS/MS analysis. The LC/MS/MS method cites two 

transition ions for each analyte in order to provide confirmation.

Method validation data, generated by PTRL West, Inc. (Hercules, CA), were included in the 

cattle feeding study. Milk was fortified with fluazinam, AMPA, and DAPA at 0.010 and 0.10 

ppm each. Muscle, liver, and kidney were fortified with the same analytes at levels of 0.01 and 

0.05 ppm each. Fat was fortified with fluazinam, AMPA, and DAPA at 0.01, 0.02, 0.1, and 0.5 

ppm each. Overall, the results showed that Method 1676W adequately recovered residues of 

fluazinam, AMPA, and DAPA in milk, muscle, and fat. Method recoveries in these matrices 

were generally within the acceptable recovery range of 70-120%. However, recoveries in liver 

and kidney were low and declined with an increase in fortification level. For hydrolyzed liver, 

overall mean recoveries of fluazinam, AMPA, and DAPA were 87%, 68%, and 38%, 

respectively, at a fortification level of 0.01 ppm. Overall mean recoveries of fluazinam, AMPA, 

and DAPA were 79%, 65%, and 34%, respectively, at a fortification level of 0.05 ppm. For 

hydrolyzed kidney, overall mean recoveries of fluazinam, AMPA, and DAPA were 96%, 75%, 

and 31%, respectively, at a fortification level of 0.01 ppm. Overall mean recoveries of 

fluazinam, AMPA, and DAPA were 63%, 39%, and 9%, respectively, at a fortification level of 

0.05 ppm. The petitioner reported that extensive method development work was performed on 

liver in an effort to obtain acceptable recoveries for DAPA residues.

An ILV of Method 1676W was performed by ADPEN Laboratories, Inc. (Jacksonville, FL) using 

two fortification levels: at the LOQ (0.01 ppm) and 10x the LOQ. Although minor 

modifications of the method for some matrices were made to make it more rugged, the ILV was 

completed within three trials. The performing laboratory concluded that, based on acceptable 

recoveries of fluazinam, AMPA, and DAPA in milk, beef fat, and beef liver down to a level of 

0.01 ppm for each compound, Method 1676W, with minor modifications, is a suitable method 

for use on bovine tissues and milk. In the first trial, the method was successfully validated for 

fluazinam and AMPA in milk, for AMPA in beef fat, and for AMPA in the liver non-hydrolysis 

procedure. In the second trial, analysis of fluazinam and DAPA in beef fat was successfully

completed after communication with the sponsor and the method developers. In the third trial, 

fluazinam, AMPA, and DAPA in milk and non-hydrolyzed liver were successfully completed 

after minor method modification.

The method was forwarded to ACB/BEAD for method validation. ACB/BEAD reported that the 

lab that performed the ILV made major modifications to the original method. As a result, HED 

requested that the registrant submit a revised method that incorporated the revisions made by the 

ILV lab. ISK Biosciences revised the method and re-submitted it. ACB/BEAD performed a 

cursory review of the revised method. The registrant incorporated the modifications made by the 

ILV lab. However, the revision eliminated the cleanup steps that were in the original method, 
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 18 of 54

and the only recovery data for the revised method were data provided by the ILV lab. 

ACB/BEAD was concerned that the elimination of the cleanup steps could lead to dirty samples 

which would, in turn, lead to analytical problems, such as interference. ACB/BEAD performed 

no further validation of the method. As the revised method contains major revisions to the 

original method, and ACB/BEAD believes it is very likely that the revised method still is not 

adequate for sample analysis or tolerance enforcement, HED recommends that the registrant 

submit an ILV for the revised method.

Conclusions. An adequate GC/ECD method (6148-91-0170-MD-001) is available for

determination of fluazinam residues in crop matrices. The method has been deemed suitable for 

tolerance enforcement because it has successfully completed the routes required for an 

enforcement method, including radiovalidation, ILV trial, and TMV trial.

An enforcement method for determination of AMGT in plants is available. AMGT is a residue 

of concern for tolerance expression in wine grapes. The registrant requested that the blueberry

submission serve as the ILV for the method. The range of fortification levels and the percent 

recovery values are acceptable. As a result, HED considers the AMGT analytical portion of the 

blueberry field trial study to be adequate, and that it can serve as the ILV for the analytical 

method for AMGT residues in plant commodities. 

At the present time, an analytical method is not available for enforcement of fluazinam tolerances 

in animal commodities. The registrant should submit an ILV of the revised method. This 

method needs to be adequate for analysis of parent fluazinam as well as the metabolites AMPA 

and DAPA in animal commodities for which tolerances will be established.

860.1360 Multiresidue Methods

Parent Fluazinam

Reference: Residue Chemistry Memo, D257115, W. Cutchin, 5/21/01

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. Data depicting the recovery of AMGT

through FDA MRMs were submitted in support of the apple petition.

Metabolite AMGT

DER Reference: 47756603.der.doc

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 
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 19 of 54

A, B, C, D, E, and F. Testing under Protocol G is not required because AMGT is not a 

substituted urea. The study was conducted by Colorado Analytical R&D Corporation (Colorado 

Springs, CO).

AMGT does not have an N-methylcarbamate structure and was not found to be naturally

fluorescent in testing under Protocol A. In Protocol B testing, the methyl ester of AMGT was not 

recovered from Florisil; therefore, no additional work was performed under Protocol B.

Protocol C testing of the compound indicated that further testing using Protocols D, E, and F was 

required for all test substances. The Protocol C results indicated that AMGT was detected using 

GC with electron capture detection (ECD) and nitrogen phosphorous detection (NPD). 

Metabolite AMGT was not recovered from grapes (non-fatty matrix) fortified at 0.05 and 0.25 

ppm using Protocol D (DB-1 column with NPD) because of matrix interference. AMGT was not 

recovered from any of the Florisil screens in Protocol E, and Protocol F testing was not 

performed. 

These data indicate that FDA multiresidue methods are not suitable for determining residues of 

the fluazinam metabolite AMGT. The submitted data will be forwarded to U.S. FDA for further 

evaluation. 

Conclusions: Adequate FDA MRM testing data are available for fluazinam and 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. Multiresidue method testing 

data are required for the regulated metabolites, AMPA and DAPA, in animals.

860.1380 Storage Stability

Residue Chemistry Memo: D257115, W. Cutchin, 5/21/01

Residue Chemistry Memo: D335640, W. Drew, 8/22/07

Plant commodities 

The storage durations and conditions of crop samples from the submitted magnitude of the 

residue and processing studies are presented in Table 7.
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 20 of 54

Table 7. Summary of Storage Conditions and Durations of Samples from Crop Field Trials. 

Matrix Storage 

Temperature (°C)

Actual Storage 

Duration (days)

Interval of Demonstrated 

Storage Stability (days) for Fluazinam

Apple, RAC -24.4 to -6.0 40-291 1,097

Apple, processed 

commodities -20 to -18 758-914 1,094-1,096

Carrot -22 to -4 450 470 1

Lettuce, head <0 64-229 419 1

Lettuce, leaf <0 42-214 419 1

Onion <-6 70-418 429 1

1 Storage stability determined from concurrent field trial samples.

The available storage stability data from previous fluazinam petitions indicate that the stability of 

fluazinam is variable under frozen conditions, depending on the crop matrix. Fluazinam has 

been found to be reasonably stable for up to 12 months in grapes and snap beans, 6.7 months in 

blueberries, and 7.6 months in broccoli. Fluazinam was also stable for up to 36 months in peanut 

nutmeats, hulls, hay, and oil, but declined by ~60% in meal after 36 months of storage. In potato 

commodities, fluazinam was stable in frozen chips for up to 18 months, but declined by 35% in 

whole potatoes and ≥70% in granules within 18 months. Residues declined by 40% in wet peel 

within 5 months. Residue declines during storage have also been observed for the following 

crops: 70% decline in cabbage by 18.3 months, 55% decline in mustard greens by 19 months, 

30% decline in ginseng by 11.4 months, 45% decline in dried beans by 10 months, and a 40% 

decline in lima beans by 15 months. To account for dissipation of residues during frozen storage, 

HED incorporated correction factors into the recommended tolerances for fluazinam residues for 

certain crop commodities.

To support the current lettuce, onion, and carrot field trial data, storage stability studies were 

conducted in conjunction with the field trials. For each crop, control samples of the respective 

matrices were fortified with fluazinam at 1.0 ppm and placed in storage under the same frozen 

conditions as the treated samples. No zero-day analyses were conducted on the fortified samples 

placed into storage. Rather, triplicate stored samples were analyzed along with a control sample 

and freshly fortified samples at an interval reflecting the maximum storage duration from the 

field trials. Average corrected recoveries of fluazinam following frozen storage were 73% from 

lettuce after 13.8 months, 86% from onions after 14.1 months, and 73% from carrots after 15.5

months. Although no 0-day analysis was conducted, the data indicate that fluazinam is stable 

under frozen storage conditions for up to 14 months in lettuce and onion and 16 months in carrot.

Storage Stability Data for Apple Fruit, Juice, and Wet Pomace

Storage stability data for fluazinam and its metabolite AMGT in apple fruit, juice, and wet 

pomace were submitted in support of the apple petition.

DER Reference: 47756604.der.doc

ISK Biosciences submitted storage stability data for fluazinam and its metabolite AMGT in apple 

fruit, juice, and wet pomace. Homogenized untreated samples of fruit, juice, and wet pomace 
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 21 of 54

were spiked with fluazinam or AMGT at 0.50 ppm, and stored frozen (-20 to -18oC) for up to 37 

months. Samples were analyzed initially (after 0 or 1 day) and following storage for 1, 2, 3, 6, 

12, 18, 30, and 36 months.

Samples of apple fruit, juice, and wet pomace were analyzed for residues of fluazinam and 

AMGT. The GC/ECD method used for fluazinam analysis is similar to the current enforcement 

method for fluazinam in crops. In addition, the HPLC/UV method used for AMGT is similar to 

the method described in “Method Evaluation for the Analysis of AMGT in Grapes” (Memo, 

D335640, W. Drew, 8/22/2007). The methods were adequate for data collection based on 

acceptable concurrent method recoveries. The reported “limit of detection” (LOD) was 0.025 

ppm for each analyte in apple fruit and wet pomace, and 0.05 ppm for each analyte in apple juice.

Residues of fluazinam appear to be relatively stable in/on apple fruit, juice, and wet pomace

stored frozen for up to 36 months. Residues of AMGT were relatively stable in/on apple fruit 

and juice stored frozen for up to 36-37 months. Residues of AMGT declined slightly in apple 

fruit to an average corrected recovery of 69% at the 36-month interval. However, AMGT 

residues in/on apple wet pomace were relatively stable for only 12 months of frozen storage. 

Residues of AMGT declined in wet pomace to an average corrected recovery of 58-63% at the 

19-month interval, 61% at the 32-month interval, and 33% at the 37-month interval.

Storage Stability Data for Cattle Milk, Meat, and Meat Byproducts

Samples collected from the dairy cow feeding study (MRID 47756605) were held under frozen 

storage conditions prior to residue analysis. The maximum storage durations of samples, from 

collection to analysis, were 146 days for milk, 185 days for cream, 179 days for skim milk, 157 

days for muscle, 203 days for fat, and 255 days for liver and kidney. A storage stability study

was conducted to validate sample storage conditions and durations. The results showed mixed 

results. In milk, cream, and skim milk, residues of fluazinam, AMPA, and DAPA were found to 

be stable for 183 days. In muscle: (i) fluazinam was stable for 1 day, but declined after 164 days 

to an average corrected recovery of 55%; (ii) AMPA was stable for 2 days, but declined after 161 

days to an average corrected recovery of 41%; and (iii) DAPA was stable for 2 days, but declined 

after 161 days to an average corrected recovery of 10%. In fat: (i) fluazinam and AMPA were 

stable for 205 days; and (ii) DAPA showed relative instability with average corrected recoveries 

of 64% after 205 days. In liver and kidney: (i) fluazinam was unstable, average recoveries in 

liver were 26-34% after 210 days, and 41-44% in kidney after 218 days; (ii) AMPA was stable in 

liver for 80/89 days, but not in kidney where average corrected recoveries were 53-58% after 218 

days; and (iii) DAPA is not stable with average corrected recoveries of 43-52% in liver after 209 

days and 17-25% in kidney after 218 days.

Conclusions. Adequate storage stability data are available to support the storage conditions and 

durations of samples collected from the magnitude of the residue studies on apples, carrots, 

lettuce, and onions. As residues of fluazinam were found to be stable in tested crop matrices, 

storage stability corrections do not need to be applied to the recommended tolerances for 

fluazinam residues in/on apples, carrots, lettuce, and onions. Storage stability data for the 

fluazinam metabolite AMGT in apple commodities were also submitted and showed that 
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 22 of 54

residues in apple wet pomace were reasonably stable for 12 months in apple wet pomace, but 

declined to an average corrected recovery of 33% at the 37-month interval. The submitted 

storage data for bovine milk, meat, and meat byproducts showed mixed results. Because of 

major data deficiencies, HED is not recommending in favor of tolerances on apple and carrot 

commodities. It is very possible that the registrant will resolve the deficiencies and re-submit the 

tolerance petitions. As a result, HED has determined the maximum reasonable dietary burdens 

for livestock based on the assumption that tolerances will be established for apples and carrots.

860.1400 Water, Fish, and Irrigated Crops

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

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 wet apple pomace and carrot culls. The livestock feedstuffs associated with registered crops 

include peanut meal and processed potato waste. 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 considered for dietary burden 

calculations. The maximum reasonable dietary burdens of fluazinam to livestock are presented 

in Table 8. The calculated dietary burdens of fluazinam are 0.04 ppm for beef cattle, 1.27 ppm 

for dairy cattle, 0.005 ppm for poultry, and 0.003 ppm for swine.

Table 8. Calculation of Dietary Burdens of Fluazinam Residues to Livestock.

Feedstuff1 Type1 % Dry 

Matter2 % Diet2 Tolerance (ppm) Dietary Contribution (ppm)

3

Beef Cattle

R not registered R -- 15 -- --

Potato, processed waste CC 15 30 0.02 0.04

CC not registered CC -- 50 -- --

PC not registered PC -- 5 -- --

TOTAL BURDEN -- -- 100 -- 0.04

Dairy Cattle

R not registered R -- 45 -- --

Apple, wet pomace CC 40 10 5.0 1.25

Potato, processed waste CC 15 10 0.02 0.013

CC not registered CC -- 25 -- --

Peanut, meal PC 85 10 0.02 0.002
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 23 of 54

Table 8. Calculation of Dietary Burdens of Fluazinam Residues to Livestock.

Feedstuff1 Type1 % Dry 

Matter2 % Diet2 Tolerance (ppm) Dietary Contribution (ppm)

3

TOTAL BURDEN -- -- 100 -- 1.27

Poultry

CC not registered CC -- 75 -- --

Peanut meal PC 85 25 0.02 0.005

TOTAL BURDEN -- -- 100 -- 0.005

Swine

CC not registered CC -- 85 -- --

Peanut meal PC 85 15 0.02 0.003

TOTAL BURDEN -- -- 100 -- 0.003

1

 R: Roughage; CC: Carbohydrate concentrate; PC: Protein concentrate.

2

 OPPTS 860.1000 Table 1 Feedstuffs (June 2008). 

3

 Contribution = ((tolerance)  (% DM)) x (% of diet) for beef and dairy cattle

 Contribution = ((tolerance) x (% of diet)) for poultry and swine.

Dairy Cattle Feeding Study

DER Reference: 47756605.der.doc

Fourteen lactating Holstein cows were divided into four treatment groups. Three groups were 

dosed orally with gelatin capsules containing fluazinam at target levels of 2.5 ppm (three cows), 

7.5 ppm (three cows), and 25 ppm (six cows) in the feed (dry weight basis) for 28 consecutive 

days. The fourth group, consisting of two cows, served as a control. Based on feed consumption 

data, the actual dosing levels were 2.91, 8.72, and 28.84 ppm. Fluazinam was weighed directly

into gelatin capsules, and the capsules were administered using a balling gun, once per day after 

the morning feeding. One control cow and three cows dosed at 25 ppm were reserved to 

investigate the depuration of residues in cow’s milk and tissues. 

Milk was collected twice daily on Days 0, 1, 3, 4, 5, 6, 7, 10, 13, 16, 19, 22, 25, and 28. In 

addition, extra milk samples from one control animal and three cows from the 2.91- and 28.84-

ppm dose groups were collected on Study Days 13 and 28 to produce data on skim milk and 

cream. Cows from the three treatment groups were sacrificed ≤ 24 hours after the final dose 

administration. One cow from the depuration group was sacrificed on Study Days 30, 32, and 

36. At sacrifice, samples of liver, kidney, fat (subcutaneous, abdominal, and perirenal), and 

muscle (leg and loin) were collected from each animal.

Samples of milk plus cream, skim milk, muscle, liver, kidney, and fat were analyzed using PTRL

Method 1676W entitled “Fluazinam, AMPA and DAPA Method in Milk and Tissues as 

Described in Magnitude of Fluazinam Residues in Bovine Tissues and Milk from a 28-Day

Feeding Study,” which was included in Appendix B of the feeding study. This method has not 

been reviewed by the PMRA or the USEPA. The method is written for LC/MS/MS analysis of 

fluazinam, AMPA, and DAPA in bovine milk and tissues, and for GC/MS analysis of DAPA in 
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 24 of 54

milk only. The method has a mild acid hydrolysis step for analysis of some matrices (milk, liver, 

and kidney) to convert the sulfamate conjugates to free AMPA and DAPA. The method limit of 

quantitation (LOQ) was 0.01 ppm for each analyte in milk and tissues. The initial validation of 

Method 1676W showed that it adequately recovered residues of fluazinam, AMPA, and DAPA 

in milk and fat. In muscle, recoveries in most were acceptable. Mean recoveries of fluazinam, 

AMPA, and DAPA at the 0.01 ppm spiking level were 82%, 96% and 90%, respectively. Mean 

recoveries of fluazinam, AMPA, and DAPA at the 0.05 ppm spiking level were 66%, 95%, and 

95%, respectively. Recoveries of AMPA and DAPA in liver and kidney were low. Recoveries 

of fluazinam from non-hydrolyzed kidney samples were also low. The results of concurrent 

method validation also showed similar low recoveries of the metabolites in liver and kidney. 

Mean recoveries of AMPA ranged from 48 to 93% in hydrolyzed liver and from 36 to 75% in 

hydrolyzed kidney. Mean recoveries of DAPA ranged from 35 to 51% in hydrolyzed liver and 

from 9 to 33% in hydrolyzed kidney. Because of low recoveries, the petitioner corrected residues 

in cow liver and kidney for concurrent method recoveries <70%. According to the petitioner, 

correspondence with ISK’s Central Institute in Japan indicates that, based on their experience 

with a variety of matrices, DAPA is easily oxidized and easily absorbed to protein and organic 

matter. This information is consistent with the observed instability and the difficulty experienced 

with recovering DAPA from some matrices. 

Samples were held under frozen storage conditions prior to residue analysis. Refer to the storage 

stability section of this memorandum for information pertaining to sample storage duration as 

well as supporting storage stability data. As Method 1676W gave very poor recovery for AMPA 

and DAPA in liver and kidney, the method needs to be revised and the feeding study needs to be 

repeated. When the feeding study is repeated, the samples need to be analyzed as soon as 

possible after sacrifice in order to minimize degradation of residues. In muscle, fluazinam 

declined by 45%, AMPA by 59%, and DAPA by 90% after 161-164 days. In fat, fluazinam and 

AMPA were stable while DAPA declined by 36% after 205 days. In liver, fluazinam declined by

as much as 74% after 210 days, AMPA was stable, and DAPA declined by 57% after 209 days. 

In kidney, fluazinam declined by 59% after 218 days, AMPA declined by 47%, and DAPA 

declined by 83% after 218 days.

The maximum residues of concern in cow milk and tissues at the dose level closest to the 

maximum reasonably balanced diet (MRBD), uncorrected and corrected for storage stability

recoveries, are summarized in Table 9. Residues in milk increased until about Day 5 and were 

essentially stable beyond that time.
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

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Table 9. Results of a Dairy Cattle Feeding Study with Fluazinam.

Matrix

Feeding 

Level 1

Maximum Uncorrected Residues for 

Storage Decline

Maximum Corrected Residues for 

Storage Decline 2

Parent AMPA DAPA Total Parent AMPA DAPA Total

Milk (Days 0-28) 8.72 <0.01 <0.01 <0.01 <0.03 -- -- -- --

Cream 28.84 <0.01 0.0582 0.1200 <0.19 -- -- -- --

Skim milk 28.84 <0.01 <0.01 <0.01 <0.03 -- -- -- --

Muscle (loin) 28.84 <0.01 0.0101 0.0179 <0.04 <0.018 <0.025 <0.179 <0.222

Muscle (round) 28.84 <0.01 <0.01 <0.01 <0.03 <0.018 <0.024 <0.100 <0.142

Liver (hydrolysis 

method)

2.91 <0.01 <0.01 <0.01 <0.03 <0.038 <0.01 <0.023 <0.071

Liver (non-hydrolysis 

method)

2.91 <0.01 <0.01 <0.01 <0.03 <0.038 <0.01 <0.023 <0.071

Kidney (hydrolysis 

method)

2.91 <0.01 <0.01 <0.01 <0.03 <0.024 <0.019 <0.059 <0.102

Kidney (nonhydrolysis method)2.91 <0.01 <0.01 <0.01 <0.03 <0.024 <0.019 <0.059 <0.102

Fat, perirenal 2.91 <0.01 <0.01 <0.01 <0.04 <0.01 <0.01 <0.016 <0.036

Fat, abdominal 2.91 <0.01 0.0169 0.0219 <0.05 <0.01 0.0169 <0.034 <0.061

Fat, subcutaneous 2.91 <0.01 <0.01 0.0107 <0.03 <0.01 <0.01 0.0167 <0.037

1

 Dose level closest to the MRBD or only dose level represented.

2 Individual residues were corrected for decline while in storage. Correcting residues for decline was made by 

dividing uncorrected residues by (100% - % decline). For milk, cream, and skim milk, no correction of individual 

residues was made. For muscle: fluazinam declined by 45%, AMPA by 59%, and DAPA by 90% after 161 days. 

For fat: fluazinam and AMPA were stable while DAPA declined by 36% after 205 days. For liver: fluazinam 

declined by as much as 74% after 210 days, AMPA was stable, and DAPA declined by 57% after 209 days. For 

kidney: fluazinam declined by 59% after 210 days, AMPA declined by 47%, and DAPA declined by 83% after 

218 days.

For the depuration study, total residues were not observed at levels higher than the combined 

LOQ (0.03 ppm) by Day 29, one day after dosing was discontinued. Total residues in tissues, 

except fat, of the animals sacrificed on Days 29, 31, and 35 after the last dose administration 

were all below the combined LOQ (0.03 ppm). In fat of animals sacrificed on Day 35, total 

residues were <0.031 ppm in perirenal fat, <0.053 ppm in abdominal fat, and <0.051 ppm in 

subcutaneous fat.

Expected Secondary Residues in Milk, Meat, and Meat Byproducts

To determine the need for tolerances for the combined residues of fluazinam, AMPA, DAPA, 

and their sulfate conjugates in milk and tissues, the anticipated secondary residues in cattle 

matrices were estimated using transfer coefficient factors calculated from the maximum 

combined residues of fluazinam observed at the dose level closest to the reasonably balanced 

dietary burden in the dairy cattle feeding study. The transfer coefficients (calculated as residue 

level to feed level ratios) are presented in Table 10. The transfer coefficient for each matrix was 

then used to calculate the expected secondary residues by multiplying the transfer coefficient by

the calculated dietary burden. The expected combined residues and the recommended tolerances 

based on expected residues are presented in Table 11.
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 26 of 54

Table 10. Residue-Level-to-Feed Ratios (Transfer Coefficients) in Dairy Cattle Milk and Tissues.

Matrix

Total Residues (Fluazinam + AMPA + DAPA, 

and Their Sulfamate Conjugates) in ppm Feeding Level

(ppm)

Transfer

Coefficient 2 Uncorrected Corrected for Storage 

Decline 1

Milk (Day 0 to Day 28) <0.03 <0.03 8.72 <0.0034

Cream <0.19 <0.19 28.84 <0.0066

Skim milk <0.03 <0.03 28.84 <0.0010

Muscle (loin) <0.04 <0.22 28.84 <0.0077

Muscle (round) <0.03 <0.14 28.84 <0.0049

Liver (hydrolysis method) <0.03 <0.07 2.91 <0.0244

Liver (non-hydrolysis method) <0.03 <0.07 2.91 <0.0244

Kidney (hydrolysis method) <0.03 <0.10 2.91 <0.0351

Kidney (non-hydrolysis 

method)

<0.03 <0.10 2.91 <0.0351

Fat, perirenal <0.04 <0.04 2.91 <0.0124

Fat, abdominal <0.05 <0.06 2.91 <0.0210

Fat, subcutaneous <0.03 <0.04 2.91 <0.0126

1 Individual residues were corrected for decline while in storage. For milk, cream, and skim milk, no correction was necessary.

2

 Calculated from the maximum corrected residues at the dose level closest to the MRBD divided by the dose level.

Table 11. Expected Total Fluazinam Residues of Concern in Meat and Milk.

Matrix Dietary Burden

(ppm)

Total Residues 1

(ppm)

Tolerance

(ppm)

Dairy Cattle

Milk (Day 0 to Day 28) 1.27 <0.0043 Not required

Cream 1.27 <0.0084 Not required

Skim milk 1.27 <0.0013 Not required

Muscle (loin) 1.27 <0.0098 Not required

Muscle (round) 1.27 <0.0062 Not required

Liver (hydrolysis method) 1.27 <0.0310 A tolerance of 0.05 ppm is 

considered to be a reasonable 

upper-bound estimate for meat 

byproducts based on expected 

residues in kidney 2.

This tolerance level is also 

considered to be a reasonable 

upper-bound estimate for fat.

Liver (non-hydrolysis method) 1.27 <0.0310

Kidney (hydrolysis method) 1.27 <0.0446

Kidney (non-hydrolysis 

method)

1.27 <0.0446

Fat, perirenal 1.27 <0.0157

Fat, abdominal 1.27 <0.0267

Fat, subcutaneous 1.27 <0.0160

Swine

Liver 0.003 0.00007 Not required

Kidney 0.003 0.00011 Not required

Muscle 0.003 0.00002 Not required

Fat 0.003 0.00006 Not required

1 Calculated from dietary burden x transfer coefficient from Table 9.

2 According to the July 18, 2007 Minutes of the Chemistry Science Advisory Council Meeting, the ChemSAC 

recommended that the guidance document be revised to include language detailing the use of the highest residue 

data for any tissue (liver, kidney, fat, skin, or muscle) to determine the tolerance for meat byproducts. A single 

tolerance on “meat byproducts” will be recommended based on that highest residue, and individual tolerances will 

no longer be set on liver, kidney, or meat byproducts (except liver and kidney).
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 27 of 54

Conclusions. Based on the poor recoveries of metabolites AMPA and DAPA from liver and 

kidney and the mixed storage stability results, the residue data from the cattle feeding study are 

not adequate to satisfy data requirements. The feeding study data (adjusted for residue decline) 

along with the calculated dietary burdens for beef cattle (0.04 ppm) and dairy cattle (1.27 ppm) 

indicate that tolerances might be needed for the combined residues of fluazinam and its 

metabolites DAPA and AMPA in the fat and meat byproducts of cattle and other ruminants at 

0.05 ppm to support the proposed use on apples. The feeding study also indicates that tolerances 

probably will not be needed for milk and meat of ruminants, as the expected combined residues 

in these matrices are below the combined method LOQ of 0.03 ppm for the regulated 

compounds. Based on the transfer coefficients for livestock tissues and the relatively low dietary

burden for swine of 0.003 ppm for fluazinam, tolerances for hogs are not needed. A poultry

feeding study is not required at this time because of low dietary burden for poultry (0.005 ppm). 

To support tolerances for apples and carrots, the registrant needs to submit a new cattle feeding 

study in which a method with better recoveries of AMPA and DAPA from liver and kidney was 

used. When this study is repeated, the samples need to be analyzed as soon as possible after 

sacrifice in order to minimize degradation of residues.

860.1500 Crop Field Trials

DER References: 47631001.der.doc (Bulb Onion)

47631002.der.doc (Leaf and Head Lettuce)

47755601.der.doc (Carrot)

47756609.der.doc (Apples: 2006 Trials)

47756606.de1.doc (Apples: 1992-1994 Trials, Includes MRIDs 47756607, 47756608, 47756610, 

and 47756611)

IR-4 and ISK Biociences Corporation have submitted magnitude of the residue studies on apples, 

carrots, lettuce, and onions. The results from these field trials are discussed below, and the 

residue data are summarized in Table 12. 

Table 11. Summary of Residue Data from Crop Field Trials with Fluazinam.

Crop Matrix Total Applic. 

Rate

(lb ai/A)

[kg ai/ha]

PHI 

(days)

Residues of Fluazinam (ppm)

1

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

Head Lettuce (proposed use = 1.0 lb ai/A total application rate, 50-day PHI)

Lettuce, head 0.952-1.02 46-52 14 <0.01 0.021 0.016 0.010 0.011 0.010

Leaf Lettuce (proposed use = 1.0 lb ai/A total application rate, 30-day PHI)

Lettuce, leaf 0.974-1.05 20-32 14 <0.01 1.690 1.570 0.021 0.260 0.010
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 28 of 54

Table 11. Summary of Residue Data from Crop Field Trials with Fluazinam.

Crop Matrix Total Applic. 

Rate

(lb ai/A)

[kg ai/ha]

PHI 

(days)

Residues of Fluazinam (ppm)

1

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

Onions (proposed use = 3.1 lb ai/A total application rate, 7-day PHI)

Onion, dry 

bulb

3.11-3.17 6-8 18 <0.01 0.101 0.098 0.014 0.027 0.028

Carrots (proposed use = 2.1 lb ai/A total application rate, 7-day PHI)

Carrot root 2.04-3.03

[2.29-3.40]

6-8 52 <0.02 0.56 0.51 0.10 0.14 0.13

Apples (proposed use = 4.5 lb ai/A total application rate, 28-day PHI)

Apples 34.44-4.77

[4.98-5.34]

28-29 24 0.02 1.75 1.75 0.15 0.38 0.58

Apples 43.97-5.40

[4.45-6.05]

28-32 16 <0.01 0.06 0.06 0.03 0.03 0.02

1

 AMGT was measured in apples and the maximum residue value for this metabolite was 0.03 ppm.

2

 HAFT = highest average field trial result.

3 Results of trials conducted during the 2006 growing season (MRID 47756609).

4

 Results of trials conducted during the 1992-1994 growing seasons (MRIDs 47756606, 47756607, 47756608, 

47756610, and 47756611).

Head and Leaf Lettuce. In fourteen field trials conducted in the United States in EPA Growing 

Zones 2, 3, and 10 during 2005-2006, 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 (DAT) for head lettuce and 20-32 DAT for 

leaf lettuce. 

Head and leaf lettuce samples were stored at ≤0°C for up to 7.6 months prior to extraction for 

analysis. The storage conditions and duration are supported by the available storage stability

data. Residues of fluazinam in/on lettuce were determined using an adequate GC/ECD method 

(6148-91-0170-MD-001, modified), which has a calculated LOQ of 0.007 ppm, and a LOD of 

0.002 ppm. The LLMV in/on lettuce was 0.01 ppm.

Following a single foliar application of fluazinam (FlC) to lettuce at a rate of 0.952-1.05 lb ai/A 

(1x), residues of fluazinam were <0.01-0.021 ppm in/on 14 head lettuce samples harvested at 46-

52 DAT, with only one sample (0.021 ppm) having residues above the LLMV. For leaf lettuce, 

residues were <0.01-1.69 ppm in/on 14 samples harvested at 20-32 DAT, with only 2 samples 

having residues <LLMV. For head lettuce, average residues were 0.011 ppm and the highest 

average field trial (HAFT) residues were 0.016 ppm. For leaf lettuce, average residues were 0.26 

ppm and the HAFT residue was 1.57 ppm. No residue decline study was conducted. In addition, 

samples were not analyzed for residues of AMGT, as required for dietary risk assessment.
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 29 of 54

Bulb Onion Subgroup (3-07A). In nine field trials conducted in the United States in EPA 

Growing Zones 1, 5, 6, 8, 10, 11, and 12 during 2005-2006, fluazinam (4.17 lb/gal FlC) was 

applied to bulb onions as six broadcast foliar applications during vegetative development and 

bulb formation at rates of 0.495-0.563 lb ai/A/application and RTIs of 5-8 days, for a total of 

3.11-3.17 lb ai/A (1x the proposed maximum seasonal rate). Applications were made using 

ground equipment in volumes of 19-60 gal/A, and no adjuvants were used. Single control and 

duplicate treated samples of onion bulbs were harvested at commercial maturity, 6-8 DAT. 

Onion bulb samples were stored at ≤-6°C for up to 13.9 months prior to extraction for analysis. 

The storage conditions and duration are supported by the available storage stability data. 

Residues of fluazinam in/on bulb onions were determined using an adequate GC/ECD method 

(6148-94-0170-MD-001, modified), which has a calculated LOQ of 0.011 ppm, and a LOD of 

0.004 ppm. The LLMV in/on onion was 0.01 ppm.

Following six broadcast foliar applications of fluazinam (FlC) to onions at rates totaling 3.11-

3.17 lb ai/A (1x), residues of fluazinam were <0.01-0.101 ppm in/on 18 onion bulb samples 

harvested at 6-8 DAT, with 7 samples having residues <0.01 ppm. Average residues were 0.027 

ppm and the HAFT residues were 0.098 ppm. In the residue decline trial, average fluazinam 

residues declined steadily from 0.085 ppm at 0 DAT to <0.01 ppm by 14 DAT.

Carrots: Thirteen carrot field trials were conducted in the United States and Canada in NAFTA 

Growing Zones 1A, 3, 5, 5B, 6, 10, and 11 during the 2005 and 2006 growing seasons. At each 

test location, Omega 500F (U.S. trials) or Allegro 500F (Canadian trials), a 4.17 lb/gal flowable 

suspension concentrate (FlC) formulation of fluazinam was applied to carrot plants as four 

broadcast or directed foliar applications (five applications were made in one trial) during 

vegetative development at rates of 0.492-0.786 lb ai/A/application (0.551-0.881 kg 

ai/ha/application) and RTIs of 6 to 9 days, for a total rate of 2.04-3.03 lb ai/A (2.30-3.40 kg ai/ha; 

1.0-1.4x the proposed maximum seasonal rate). Applications were made using ground 

equipment in volumes of 24-60 gal/A (220-560 L/ha), and no adjuvants were used. One 

untreated plot and two treated plots were used at each site. Each treated plot received treatments 

in similar rates and volumes; however, one treated plot was irrigated within two hours of each 

application, and the other treated plot received no irrigation for at least 24 hours after each 

application. Duplicate treated and untreated samples of carrot root were harvested at commercial 

maturity at a 6- to 8-day PHI. Additional samples were harvested at 1, 13, and 20-day PHIs at 

the Reverside, CA trial site to assess residue decline behavior.

Samples of carrot root were stored frozen for up to 450 days (14.8 months) between harvest and 

analysis. Concurrent storage stability data were provided demonstrating the relative stability of 

fluazinam in/on carrot root for up to 470 days (15.5 months) of frozen storage. However, zeroday data were not provided. Storage stability studies should always include a zero-day sampling 

interval to establish the residue levels present at the time samples are placed into storage (see 

OPPTS 860.1380(d)(6)(i)).

Residues of fluazinam in carrot root samples were determined using the gas chromatography/ 

electron capture detection (GC/ECD) Method YARL-0605A (Method No. 94-017 in PMRA 
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 30 of 54

#1407042). The modified method was adequate for data collection based on acceptable method 

validation and concurrent recoveries. The validated limit of quantitation (LOQ; or the LLMV) 

was 0.02 ppm. The calculated LOQ was 0.024 ppm. The calculated limit of detection (LOD) 

was 0.0081 ppm.

Following four foliar applications of the 4.17 lb/gal FlC formulation of fluazinam to carrots at 

total rates of 2.04-2.94 lb ai/A (2.29-3.29 kg ai/ha; 1.0-1.4x application rates) with irrigation 

within 2 hours of the last application, residues of fluazinam ranged <0.02-0.56 ppm in/on 26 

carrot root samples harvested at a 6- to 8-day PHI. Residues of fluazinam ranged from <0.02-

0.45 ppm following applications at 2.04-3.03 lb ai/A (2.29-3.40 kg ai/ha; 1.0-1.4x) with 

irrigation withheld for at least 24 hours following the last application. Fluazinam residues from 

each treatment pattern were comparable: the average residues for carrot samples receiving 

irrigation within 2 hours or after 24 hours of the final application were 0.15 and 0.12 ppm, 

respectively, and the HAFT residues were 0.51 and 0.43 ppm, respectively. In the residue 

decline trial, average residues of fluazinam in/on carrot roots declined from the 1-to the 8-day

PHI (from 0.67 to 0.15 ppm), increased at the 13-day PHI (0.36 ppm) and declined slightly at the 

20-day PHI (0.34 ppm) for the early-irrigation treatment pattern. For the late-irrigation treatment 

pattern, average residues declined from the 1- to the 8-day PHI (from 0.53 to 0.21 ppm), 

increased at the 13-day PHI (0.45 ppm), then declined again at the 20-day PHI (0.33 ppm).

Apples (MRID 47756609): Twelve apple field trials were conducted in the United States and 

Canada in NAFTA Growing Zones 1, 5A, 5B, 9, 10, and 11 during the 2006 growing season. At 

each test location, consisting of one untreated and one treated plot, a 4.17 lb/gal FlC formulation 

of fluazinam was applied to apple trees (ages 5-38 years) as ten airblast foliar applications during 

fruit development at rates of 0.435-0.713 lb ai/A/application (0.488-0.799 kg ai/ha/application) 

and RTIs of 6 to 8 days, for a total rate of 4.44-4.77 lb ai/A (4.98-5.34 kg ai/ha). The identical 

product was used in both the U.S. and Canadian trials. In the U.S., the name of this product is 

Omega 500F, and in Canada, the name of this product is Allegro 500 F. Applications were made 

using ground equipment (tractor or backpack sprayer) in volumes of 51-152 gal/A (480-1420 

L/ha), and no adjuvants were used. Duplicate treated and untreated samples of apple fruit were 

harvested at commercial maturity at a 28- or 29-day PHI. At two trials, additional samples were 

harvested at 0-, 7-, 14-, and 21-day PHIs to evaluate residue decline.

Samples of apple fruit were stored frozen for up to 144 days (4.7 months) between harvest and 

analysis. Adequate storage stability data are available (refer to the DER for MRID 47756604) for 

fluazinam and AMGT to support the storage conditions and durations of apple samples discussed 

in this summary document. These data indicate that residues of fluazinam and AMGT appear to 

be relatively stable under frozen storage in apple fruit for up to 36 months. 

The GC/ECD method used for fluazinam analysis is similar to the current enforcement method 

for fluazinam in crops. In addition, the HPLC/UV method used for AMGT is similar to the 

method described in “Method Evaluation for the Analysis of AMGT in Grapes” (Memo, 

D335640, W. Drew, 8/22/2007). The methods used for fluazinam and AMGT were adequate for 

data collection based on acceptable method validation and concurrent recovery data. The 

validated LOQ was 0.01 ppm for each analyte in apple fruit; the calculated LOQs were 0.011 and 
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 31 of 54

0.017 ppm, respectively, for fluazinam and AMGT. The calculated LODs were 0.0031 and 

0.0055 ppm for fluazinam and AMGT, respectively, in apple fruit.

Following ten foliar airblast applications of the 4.17 lb/gal FlC formulation of fluazinam to 

apples at total rates of 4.44-4.77 lb ai/A (4.98-5.34 kg ai/ha; 1.0-1.1x), maximum residues of 

fluazinam were 1.75 ppm and maximum residues of AMGT were 0.03 ppm. In the residue 

decline trials, residues of fluazinam in/on apple fruit declined from the 0- and 7-day PHIs to the 

28- or 29-day PHI. In one trial, the 0-day samples were not analyzed.

Apples (MRIDs 47756606, 47756607, 47756608, 47756610, and 47756611): Eight apple field 

trials were conducted in the United States and Canada in NAFTA growing Zones 1, 1A, 2, 5, and 

5A during the 1992, 1993, and 1994 growing seasons. Three additional trials were conducted in 

Zones 10 (CA; 1 trial) and 11 (WA; 2 trials); however, these trials were conducted at lower total 

application rates (2.17-3.15 lb ai/A) and a longer PHI (90 days). At each test location, consisting 

of one untreated plot and one treated plot, a 4.17 lb/gal FlC formulation of fluazinam was applied 

to apple trees (ages 6-30 years) as 9 to 12 (5 to 7 for the WA and CA trials) airblast foliar 

applications during fruit development at rates of 0.43-0.48 lb ai/A/application (0.48-0.54 kg 

ai/ha/application) and RTIs of 7 to 23 days. The total application rates ranged from 3.97-5.40 lb 

ai/A (4.45-6.05 kg ai/ha; 0.9-1.2x the proposed maximum seasonal rate). At the other three 

trials, 5 to 7 airblast foliar applications were made at rates of 0.43-0.45 lb ai/A/application (0.48-

0.50 kg ai/ha/application) and RTIs of 4 to 15 days, for a total rate of 2.17-3.15 lb ai/A (2.43-3.53

kg ai/ha). Applications were made using ground equipment (tractor-mounted sprayer) in 

volumes of 72-184 gal/A (673-1721 L/ha), and no adjuvants were used. Two additional plots 

were established at the PA site, one treated at a low spray volume (~20-21 gal/A (191-197 L/ha))

and the other at twice the nominal rate (0.9 lb ai/A (1.0 kg ai/ha)) and a dilute spray volume 

(195-198 gal/A (1824-1852 L/ha)). Duplicate treated and untreated samples of apple fruit were 

harvested at commercial maturity at a 28- to 32-day PHI.

Samples were stored frozen for up to 291 days (9.6 months) prior to determination of residues of 

fluazinam. For AMGT analysis, four samples from the 1992 trials were stored frozen for up to 

1189 days (39.1 months) and twenty-two samples from the 1993-1994 trials were stored frozen 

up to 797 days (26.2 months). The submitted storage stability data for fluazinam and AMGT are 

adequate to support the storage durations and conditions of samples from the apple field trials

(refer to the DER for MRID 47756604). Although apple samples from the 1992 trials were 

stored longer than 36 months prior to AMGT analysis, the submitted storage stability data are 

adequate to support the storage durations and conditions of samples from the apple field trials as 

the majority of samples were stored less than 36 months, and residues in these samples are 

comparable.

The GC/ECD method used for fluazinam analysis is similar to the current enforcement method 

for fluazinam in crops. In addition, the HPLC/UV method used for AMGT is similar to the 

method described in “Method Evaluation for the Analysis of AMGT in Grapes” (Memo, 

D335640, W. Drew, 8/22/2007). The methods used for fluazinam and AMGT were adequate for 

data collection based on acceptable method validation and concurrent recovery data. The 

validated LOQ was 0.01 ppm for each analyte in apple fruit.
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

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Following 9 to 12 foliar airblast applications of the 4.17 lb/gal FlC formulation of fluazinam to 

apples at total rates of 3.97-5.40 lb ai/A (4.45-6.05 kg ai/ha), maximum residues of fluazinam 

were 0.08 ppm and maximum residues of AMGT were 0.02 ppm. Residue decline data were not 

generated for these trials, but are available in the 2006 apple field trial data (refer to the DER for 

MRID 47756609).

In the PA trial performed at a total application rate of 9.0 lb ai/A (10.1 kg ai/ha), the fluazinam 

residue levels were 0.08 and 0.10 ppm and the AMGT residue levels were 0.01 and <0.01 ppm.

Bushberry subgroup 13-07B. IR-4 submitted a request to revise the established 7.0-ppm 

tolerances for fluazinam residues in/on the Bushberry subgroup 13B and other bushberry type 

crops (aronia berry, buffalo currant, Chilean guava, European barberry, highbush cranberry, 

edible honeysuckle, jostaberry, Juneberry, lingonberry, native currant, salal, sea buckthorn). 

These tolerances were originally established under PP# 6E7137 (Memo, D335640, W. Drew,

8/22/07). IR-4 is requesting that a single tolerance be established for the Bushberry subgroup 13-

07B for residues of fluazinam at a level of 4.5 ppm. 

No new residue data were submitted in support of the tolerance amendment request. The original 

blueberry residue data for fluazinam per se were entered into the tolerance spreadsheet. HED 

concludes that the residue data for fluazinam from the blueberry field trials are distributed 

lognormally. Therefore, the recommended tolerance for the bushberry subgroup is 7.0 ppm, 

which is equivalent to the current tolerance for blueberries. Therefore, the recommended 

tolerance for the revised Bushberry subgroup 13-07B is also 7.0 ppm.

Conclusions. With the exception of the use of adjuvants (see 860.1200), the submitted field trial 

data for fluazinam on head lettuce, leaf lettuce, bulb onions, carrots, and apples are acceptable 

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

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

collected from each test at, or close to, the proposed PHI. Samples from all the field trials were 

analyzed for fluazinam residues using an adequate GC/ECD method, and the storage stability

data support the sample storage durations for these crops. However, no residue data were 

provided on AMGT residues in lettuce. Although, AMGT residue data on lettuce are still 

required for purposes of dietary risk assessment, the available data support tolerances of 0.02 

ppm for head lettuce, 2.0 ppm for leaf lettuce, 0.20 ppm for the bulb onion (Subgroup 3-07A), 

1.7 ppm for apple, and 0.7 ppm for carrot. For dietary risk assessment, HED will calculate 

AMGT residues in lettuce using a ratio of 0.35:1 for AMGT:fluazinam residues (ChemSAC 

Memo, meeting of 2/6/08). However, the samples from the lettuce field trials still need to be 

analyzed for residues of AMGT.

After reevaluating the available residue data for blueberries, HED concludes that the residue data 

for fluazinam from the blueberry field trials are distributed lognormally. Therefore, the 

recommended tolerance for the Bushberry subgroup 13-07B is 7.0 ppm.
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860.1520 Processed Food and Feed

DER Reference: 47756606.de2.doc (Includes MRIDs 47756610 and 47756611)

Apples: In a single crop field trial conducted in NY during the 1993 growing season, a 4.17 

lb/gal FlC formulation of fluazinam was applied to mature apple trees as ten foliar airblast 

applications at a rate of 0.45 lb ai/A/application (0.50 kg ai/ha/application), with 7- to 14-day

RTIs, for a total rate of 4.50 lb ai/A (5.04 kg ai/ha; 1x the proposed maximum seasonal rate). 

The first application was made when fruit development was at the green tip growth stage, with 

subsequent applications being made up to 6.3-6.6 cm diameter fruit, and all applications were 

made using ground equipment in 99-104 gal/A (926-973 L/ha) volumes without an adjuvant. 

Mature apples were collected at a 29-day PHI and processed into wet and dry apple pomace, raw 

apple juice, and apple cider.

Samples of whole apples and processed commodities were analyzed for residues of fluazinam 

and AMGT. The GC/ECD method used for fluazinam analysis is similar to the current 

enforcement method for fluazinam in crops. In addition, the HPLC/UV method used for AMGT 

is similar to the method described in “Method Evaluation for the Analysis of AMGT in Grapes.” 

These methods were reviewed under DP# 335640, W. Drew, 8/22/07. These methods are

adequate for data collection based on acceptable method verification and concurrent method 

recoveries. The fortification levels used in method verification and concurrent method validation

were adequate to bracket expected residue levels in/on apple fruits, the raw agricultural 

commodity (RAC), wet and dry pomace, juice, and cider. The validated method LOQ was 0.01 

ppm for each analyte in all matrices.

Samples of apple fruits were stored frozen for up to 191 days (6.3 months) prior to determination 

of residues of fluazinam and 805 days (26.4 months) prior to determination of residues of 

AMGT. Samples of processed commodities were stored frozen for 194-236 days (6.4-7.8 

months) prior to fluazinam analysis and for 758-914 days (24.9-30.0 months) prior to AMGT 

analysis. The submitted storage stability data (refer to the DER for MRID 47756604) for 

fluazinam and AMGT are adequate to support the storage durations and conditions of samples 

from the apple processing study.

The results of the apple processing study are summarized in Table 13. Average residues of 

fluazinam and AMGT were 0.025 ppm and below the LOQ (<0.01 ppm), respectively, in/on 

apple fruit (RAC) harvested 29 days following foliar airblast treatments with the 4.17 lb/gal FlC 

formulation at a 1x application rate. Respective average residues of fluazinam and AMGT were 

0.07 and <0.01 ppm in wet pomace; 0.09 and 0.01 ppm in dry pomace; and <0.01 ppm each in 

both raw juice and cider. In the processing study, residues of fluazinam concentrated in wet 

pomace (2.8x) and dry pomace (3.6x), but did not concentrate in juice or cider (<0.4x in each 

matrix). Residues of AMGT did not concentrate in dry pomace (1x). Processing factors were 

not calculated for AMGT in wet pomace, juice, or cider as the observed residues were <LOQ in 

both the RAC and the processed commodity. The observed processing factors are less than the 

theoretical concentration factor of 14x for wet apple pomace (OPPTS 860.1520, Table 4).
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

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Table 13. Residue Data from Apple Processing Study with Fluazinam.

Location

(City, State; Year)

Total Rate

(lb ai/A) 

[kg ai/ha]

PHI 

(days)

Commodity Fluazinam 

residues

(ppm)

[Avg.]

Fluazinam 

Processing 

Factor

AMGT 

residues

(ppm)

[Avg.]

AMGT 

Processing 

Factor1

Williamson, NY; 1993 4.50

[5.04]

29 Fruit (RAC) 0.03, 0.02

[0.025]

-- <0.01, <0.01

[<0.01]

--

Wet pomace 0.07, 0.07

[0.07]

2.8x <0.01, <0.01

[<0.01]

NC

Dry pomace 0.10, 0.08

[0.09]

3.6x 0.012, 0.012

[0.01]

1x

Raw juice <0.01, <0.01

[<0.01]

<0.4x <0.01, <0.01

[<0.01]

NC

Cider <0.01, <0.01, 

<0.01

[<0.01]

<0.4x <0.01, <0.01, 

<0.01

[<0.01]

NC

1

 NC = Not calculated; residues were below the LOQ (<0.01 ppm) in both the RAC and the processed fraction.

Conclusions: The apple processing study is not adequate to satisfy data requirements. In apples, 

the metabolite AMGT is a residue of concern for risk assessment. In the processing study there 

were no quantifiable residues of AMGT in raw apples. In several of the field trials that were 

performed, however, raw apples contained AMGT residues at, or above, the limit of quantitation. 

In a few cases, residues of AMGT were comparable to those of the parent fluazinam. Canadian 

and U.S. residue chemistry guidelines both stipulate that in the processing study, if residues in 

the raw agricultural commodity (RAC) are below the LOQ, but quantifiable residues occurred in 

the RAC in field trials performed at the maximum requested label rate, that the processing study

should be conducted at exaggerated rates in order to ensure that quantifiable residues will be 

present in the RAC. Quantifiable residues are needed in the RAC in order to determine a reliable 

concentration factor. As a result, the processing study needs to be repeated at a sufficiently high 

rate that residues of both parent and AMGT are quantifiable in the RAC. In the event that the 

potential for phytotoxicity exists, the application rate does not need to be greater than the rate at 

which phytotoxicity occurs.

860.1650 Submittal of Analytical Reference Standards

Analytical reference standards for fluazinam (expiration date 4/12/2012) AMPA (expiration date 

5/31/2011), and DAPA (expiration date 4/2012) are currently available in the EPA National 

Pesticide Standards Repository (electronic communication D. Wright, ACB, to D. Dotson, HED, 

11/18/2009). An analytical standard for the AMGT metabolite is not currently available in the 

EPA National Pesticide Standards Repository. The standard 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.
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

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860.1850/1900 Confined and Field Accumulation in Rotational Crops

Residue Chemistry Memo DP#s 212612, 216941, and 217467; 9/5/95; G. Herndon

Residue Chemistry Memo DP# 342005, 2/1/08, W. Drew

An adequate confined rotational crop study is available in which barley, carrots, and lettuce were 

grown in soil treated with [phenyl-U14C]fluazinam or [pyridyl-2,6-

14C]fluazinam at 2.0 lb ai/A. 

All three crops were planted at PBIs of 30, 120, and 365 days, and no crops were grown in the 

soil during the aging period. Because of crop failure, the 30-day PBI barley in the plot treated 

with [phenyl-U14C]fluazinam was replanted at a 68-day PBI. 

Although total radioactive residues (TRR) were greater than 0.01 ppm in/on all rotational crop 

RACs (except 365-day PBI pyridine-labeled carrot roots), no fluazinam or any other metabolite 

resembling the intact fluazinam molecule was detected in any rotational crop RAC, from even 

the shortest rotation interval (30-68 days). The majority of the radioactivity was found in the 

aqueous soluble fractions of plant extracts, although some of the barley samples exhibited a high 

percentage of bound radioactivity. The organic fraction of each crop matrix contained <10% or 

<0.01 ppm of the TRR. Radioactivity in aqueous fractions accounted for up to 75-95% of the 

TRR (0.06-0.27 ppm) in phenyl-labeled crops, and up to 27-60% (0.02-0.046 ppm) in pyridyllabeled crops. Analysis of the phenyl-labeled aqueous fractions indicated that the majority of the 

radioactivity eluted early (4-5 minutes) in a single band which was identified as TFA. The 

pyridine-labeled aqueous fractions exhibited late-eluting radioactivity (15-20 minutes), indicating 

different metabolism pathways between the two labels. No metabolites from the pyridine-labeled 

aqueous fractions were identified.

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. HED originally recommended that labels specify

rotational crop restrictions of 70 days for cereal grain and 30 days for all other crops. However, 

in a recent reexamination of the data (Memo, D342005, W. Drew, 2/01/08), HED concluded that 

a 30-day PBI is sufficient for all rotated crops not on the label. No additional rotational crop data 

are required for the proposed uses on carrots, lettuce, and onions.

860.1550 Proposed Tolerances

For purposes of tolerance expression, HED previously determined that the residue of concern is 

fluazinam per se for all plant commodities, except for wine grapes where the parent compound 

and the metabolite AMGT are the residues of concern. For poultry and ruminants, the fluazinam 

residues of regulatory interest include the parent plus the metabolites AMPA and DAPA, and 

their sulfamate conjugates.

Tolerances for residues of fluazinam are listed under 40 CFR §180.574. Permanent tolerances 

have been established for residues of fluazinam in/on plant commodities at levels ranging from 

0.01 ppm on turnip greens and Brassica leafy vegetables to 7.0 ppm in/on the Bushberry

subgroup and other bushberries (40 CFR §180.574(a)(1)). A tolerance without a U.S. 
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 36 of 54

registration has also been established for residues of fluazinam and its metabolite AMGT in/on 

wine grapes at 3.0 ppm (40 CFR §180.574(a)(2)).

The tolerance expression proposed by IR-4 in PP#8E7506 and PP#9E7570 for head lettuce, leaf

lettuce, carrots, and the Bulb onion Subgroup (3-07A), is in terms of fluazinam. The tolerance 

expression proposed by ISK Biosciences in PP#9F7571 for apples and apple wet pomace is in 

terms of the combined residues of fluazinam and its metabolite AMGT. However, only the 

parent needs to be regulated for these commodities. Parent and AMGT are the residues of 

concern for risk assessment, but not for tolerance expression. As a result, if and when ISK 

Biosciences resubmits the tolerance petition for apples, the tolerance expression for apples and 

apple wet pomace should be defined as fluazinam only. The tolerance expression proposed by

ISK Biosciences in PP# 9F7571 for milk, meat, and meat byproducts is appropriate and 

adequately reflects the combined residues of fluazinam and its metabolites DAPA and AMPA.

HED recommends that 40CFR §180.574(a)(1) be amended by replacing the tolerance expression 

with the following: “Tolerances are established for residues of fluazinam (3-chloro-N-[3-chloro2,6-dinitro-4-(trifluoromethyl)phenyl]-5-(trifluoromethyl)-2-pyridinamine), including its 

metabolites and degradates, in or on the commodities in the table below. Compliance with the 

tolerance levels specified below is to be determined by measuring only fluazinam.” HED further 

recommends that 40CFR §180.610(a)(2) be amended by replacing the tolerance expression with 

the following: “Tolerances are established for residues of fluazinam, including its metabolites 

and degradates, in or on the commodities in the table below. Compliance with the tolerance 

levels specified below is to be determined by measuring only fluazinam and its metabolite 

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

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

Adequate numbers of field trials at ~1x the proposed use rate are available for head lettuce, leaf 

lettuce, bulb onions, carrots, and apples to support permanent tolerances on these crops. With 

the exception of head lettuce, the Agency’s SOP “Guidelines for Setting Pesticide Tolerances 

Based on Field Trial Data” were utilized for determining the appropriate tolerance level for each 

commodity (Appendix II). The recommended tolerances for these crop commodities are listed in 

Table 14. For head lettuce, the tolerance spreadsheet could not be used to calculate a possible 

tolerance because of the large number of residue values <LOQ (13 of 14 samples). Therefore, 

the maximum residue value (0.021 ppm) was used to determine the appropriate tolerance for 

head lettuce of 0.02 ppm.

IR-4 has requested that the Agency reconsider the established 7-ppm tolerances for members of 

the Bushberry subgroup 13B, as the established tolerances are 3.5 times as high as the maximum 

residue value. IR-4 has also requested deletion of the separate tolerances for bushberry crops that 

are now covered by the updated Bushberry subgroup 13-07B. The existing blueberry residue 

data for fluazinam were reevaluated according to the Agency’s SOP “Guidelines for Setting 

Pesticide Tolerances Based on Field Trial Data.” After reviewing the probability plot for the 

fluazinam residue data on blueberries, HED has determined that the residue data are lognormally

distributed, and that the recommended tolerance for the Bushberry subgroup 13-07B should be 
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 37 of 54

7.0 ppm. In addition, the separate tolerances for the various bushberry crops can now be deleted, 

as all of the listed bushberries are now covered by the revised Bushberry subgroup 13-07B.

The apple processing study is not acceptable. In apples, the metabolite AMGT is a residue of 

concern for risk assessment. In the processing study there were no quantifiable residues of 

AMGT in raw apples. In several of the field trials that were performed, however, raw apples 

contained AMGT residues at, or above, the limit of quantitation. In a few cases, residues of 

AMGT were comparable to those of the parent fluazinam. Canadian and U.S. residue chemistry

guidelines both stipulate that in the processing study, if residues in the raw agricultural 

commodity (RAC) are below the LOQ, but quantifiable residues occurred in the RAC in field

trials performed at the maximum requested label rate, that the processing study should be 

conducted at exaggerated rates in order to ensure that quantifiable residues will be present in the 

RAC. Quantifiable residues are needed in the RAC in order to determine a reliable concentration 

factor. As a result, the processing study needs to be repeated at a sufficiently high rate that 

residues of both parent and AMGT are quantifiable in the RAC. In the event that the potential 

for phytotoxicity exists, the application rate does not need to be greater than the rate at which 

phytotoxicity occurs.

The residue data (adjusted for residue decline) from the cattle feeding study, along with the 

calculated dietary burdens for beef and dairy cattle, indicate that tolerances might be needed for 

the combined residues of fluazinam and its metabolites DAPA and AMPA in fat and meat

byproducts of cattle and other ruminants at 0.05 ppm. The feeding study also indicates that 

tolerances probably will not be needed for milk and meat of cattle and ruminants, as the expected 

combined residues in these matrices are below the combined method LOQ of 0.03 ppm for the 

regulated compounds. According to the July 18, 2007 Minutes of the Chemistry Science 

Advisory Council Meeting, the ChemSAC recommended that the guidance document be revised 

to include language detailing the use of the highest residue data for any tissue (liver, kidney, fat, 

skin or muscle) to determine the tolerance for meat byproducts. A single tolerance on “meat 

byproducts” would be recommended based on the highest residue value, and individual 

tolerances will no longer be set on liver, kidney, or meat byproducts (except liver and kidney).

Based on the transfer coefficients for livestock tissues and the relatively low dietary burden for 

swine of 0.003 ppm for fluazinam, tolerances for hogs are not needed. Tolerances are also not 

needed for poultry eggs and tissues at this time because of the low dietary burden for poultry. 

Tolerances for rotational crops are not required based on the review of a confined rotational crop 

study which showed the absence of metabolites containing the intact fluazinam nucleus. The 

existing 30-day PBI for all rotated crops not on the label is appropriate, and precludes the need 

for additional rotational crop data.
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 38 of 54

There are currently no established Codex, Canadian, or Mexican maximum residue limits 

(MRLs) for fluazinam on the apple, carrot, lettuce, onions or berry crops. Therefore, there are no 

harmonization issues for the requested tolerances. An International Residue Limit Status Sheet is 

attached in Appendix I.

Table 14. Tolerance Summary for Fluazinam.

Commodity

Proposed 

Tolerance 

(ppm)

Recommended 

Tolerance (ppm)

Comments; Correct Commodity Definition

PP#8E7506

Bushberry, subgroup 13-07B 4.5 7.0 Adequate blueberry residue data are available. 

The recommended tolerance for Subgroup 13-07B 

is the same as that for Subgroup 13B (i.e., 7.0 

ppm)

The established individual tolerances for aronia 

berry, buffalo currant, Chilean guava, European 

barberry, highbush cranberry, edible honeysuckle,

edible jostaberry, Juneberry, lingonberry, native

currant, salal, and sea buckthorn should be deleted 

because they are included under the revised 

Bushberry subgroup, 13-07B.

Onion, bulb, subgroup 3-07A 0.15 0.20 Adequate bulb onion residue data are available.

Lettuce, head 0.02 0.02 Adequate head lettuce residue data are available.

Lettuce, leaf 2.0 2.0 Adequate leaf lettuce residue data are available.

PP#9E7570

Carrot, roots 0.8 None Adequate carrot residue data are available. 

HED’s tolerance generator directs that the 

tolerance for this data set should be 0.70 ppm. 

PP#9F7571

Apples 1.7 None Adequate apple residue data are available. HED’s 

tolerance generator directs that the tolerance for 

this data set should be 1.50 ppm. The USEPA and 

Canada’s PMRA agreed to establish the tolerance 

at 2.0 ppm at such time as the data deficiencies are 

resolved.

Apple, pomace, wet 5.0 None Adequate apple processing data are not available.

Cattle, fat 0.03 None An adequate cattle feeding study is not available. 

Based on the results of the inadequate study, the 

maximum expected residues in meat byproducts 

and fat is 0.05 ppm. This value can be used as a 

very conservative residue value for the dietary 

exposure assessment.

Based on the results of the inadequate feeding 

study, tolerances will probably not be needed for 

milk and meat of cattle, goat, horse, and sheep.

Cattle, kidney 0.03 Not required

Cattle, liver 0.03 Not required

Cattle, meat 0.03 Not required

Cattle, meat byproducts 0.03 None

Goat, fat 0.03 None

Goat, kidney 0.03 Not required

Goat, liver 0.03 Not required

Goat, meat 0.03 Not required

Goat, meat byproducts 0.03 None

Horse, fat 0.03 None
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 39 of 54

Table 14. Tolerance Summary for Fluazinam.

Commodity

Proposed 

Tolerance 

(ppm)

Recommended 

Tolerance (ppm)

Comments; Correct Commodity Definition

Horse, kidney 0.03 Not required

Horse, liver 0.03 Not required

Horse, meat 0.03 Not required

Horse, meat byproducts 0.03 None

Milk 0.03 Not required

Sheep, fat 0.03 None

Sheep, kidney 0.03 Not required

Sheep, liver 0.03 Not required

Sheep, meat 0.03 Not required

Sheep, meat byproducts 0.03 None

References

D212612, 216941, and 217467, PP# 2G04099. Temporary Tolerance Petition and Experimental 

Use Permit for Use of Fluazinam on Peanuts; 050534-EUP-E. Submission Dated 1/23/95 in 

Response to the Memo of G.J. Herndon Dated 6/19/92, G. Herndon, 9/5/95

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

Cutchin, 4/23/01

D257115, PP# 9F5079. Request for the Use of Fluazinam on Peanuts, Potatoes, and Wine 

Grapes. Evaluation of Analytical Chemistry and Residue Data, W. Cutchin, 5/21/01

D335640, Fluazinam. Tolerance Petitions Requesting the Establishment of Permanent

Tolerances (Associated with Section 3 Registration) for Food Use of the Fungicide on EdiblePodded Beans (Subgroup 6-A, Except Peas), Shelled Succulent Beans (Subgroup 6-B, Except 

Peas), Shelled Dried Beans (Subgroup 6-C, Except Peas), Brassica (Cole) Vegetables (Group 5), 

Bushberries (Subgroup 13-B), and Ginseng. Summary of Analytical Chemistry and Residue 

Data, W. Drew, 8/22/07

D342005, Fluazinam. Request for Label Amendments Adding Aerial Application of the 

Fungicide on Potatoes, and Reducing the Plant-Back Interval (PBI) for All Non-Label Crops 

from 70 to 30 Days Following Use of the Fungicide, W. Drew, 2/1/08

Attachments: 

Appendix I - International Residue Limit Status sheet

Appendix II - Tolerance Assessment Calculations
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 40 of 54

Appendix I

INTERNATIONAL RESIDUE LIMIT STATUS

Chemical Name: 3-chloroN-[3-chloro-2,6-dinitro-4-

(trifluoromethyl)phenyl]-5-

(trifluoromethyl)-2-

pyridinamine

Common Name: 

Fluazinam

X Proposed tolerances

⁯ Reevaluated tolerance

⁯ Other

Date: 8/31/09

Codex Status (Maximum Residue Limits) U. S. Tolerances

√ No Codex proposal step 6 or above

⁯No Codex proposal step 6 or above for the crops 

requested

Petition Numbers: PP#s 8E7506, 9E7570, and 9F7571

DP #s: 360840 and 366506

Other Identifier: 

Residue definition (step 8/CXL): N/A Reviewer/Branch: C. Swartz, RAB2

Established residue definition: parent fluazinam for all 

plant commodities, except wine grapes; parent 

fluazinam and AMGT for grapes

Proposed residue definition in PP#s 8E7506 and 

9E7570 for plant commodities: fluazinam

Proposed residue definition in PP#9F7571 for apple 

commodities: fluazinam and its metabolite AMGT and 

for livestock commodities: fluazinam and its 

metabolites DAPA and AMPA

Crop (s) MRL (mg/kg) Crop(s) Proposed

Tolerance (ppm)

PP#8E7506; fluazinam

Bushberry, subgroup 13-07B 4.5

Onion, bulb, subgroup 3-07A 0.15

Lettuce, head 0.02

Lettuce, leaf 2.0

PP#9E7570; fluazinam

Carrot, roots 0.8

PP#9F7571; fluazinam and AMGT

Apple 1.7

Apple, pomace, wet 5.0

PP#9F7571; fluazinam and its metabolites DAPA 

and AMPA

Cattle, fat 0.03

Cattle, kidney 0.03

Cattle, liver 0.03

Cattle, meat 0.03

Cattle, meat byproducts 0.03
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 41 of 54

Goat, fat 0.03

Goat, kidney 0.03

Goat, liver 0.03

Goat, meat 0.03

Goat, meat byproducts 0.03

Horse, fat 0.03

Horse, kidney 0.03

Horse, liver 0.03

Horse, meat 0.03

Horse, meat byproducts 0.03

Milk 0.03

Sheep, fat 0.03

Sheep, kidney 0.03

Sheep, liver 0.03

Sheep, meat 0.03

Sheep, meat byproducts 0.03

Limits for Canada Limits for Mexico

⁯No Limits

√ No Limits for the crops requested

⁯ No Limits

√ No Limits for the crops requested

Residue definition: 3-chloro-N-[3-chloro-2,6-dinitro-4-

(trifluoromethyl)phenyl]-5-(trifluoromethyl)-2-

pyridinamine

Residue definition: Fluazinam

Crop(s) MRL (mg/kg) Crop(s) MRL (mg/kg)

Potatoes 0.02 Beans 0.1

Potato 0.05

Notes/Special Instructions: S. Funk, 09/02/2009
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 42 of 54

Appendix II

Tolerance Assessment Calculations

For each of the crops listed below, the Guidance for Setting Pesticide Tolerances Based on Field 

Trial Data (SOP), along with the tolerance spreadsheet (January 2008 version), was used for 

calculating recommended tolerances. As specified in the SOP, the minimum of the 95% upper 

confidence limit (UCL) on the 95th percentile and the point estimate of the 99th percentile was 

selected as the tolerance value in cases when the dataset was large (greater than 15 samples) and 

reasonably lognormal. For datasets that were small (≤15 samples) and reasonably lognormal, the 

upper bound estimate of the 95th percentile based on the median residue value was compared to 

the minimum of the 95% UCL on the 95th percentile and the point estimate of the 99th 

percentile, and the minimum value was selected as the tolerance value. For datasets that were 

not lognormal, the upper bound on the 89th percentile was selected as the tolerance value 

(distribution-free method). The rounding procedures specified in the SOP were also used.

Apple

The dataset used to establish a tolerance for fluazinam on apple consisted of field trial data 

representing application rates of 3.97-5.40 lb ai/A (9-12 applications at 0.43-0.71 lb 

ai/A/application) with PHIs of 28-32 days. As specified in the SOP, the trial application rates

and PHIs are within 25% of the maximum label application rate and minimum label PHI, 

respectively. The residue values used to calculate the tolerance for apple are provided in Table 

II-1.

All but 4 of the 42 field trial sample results for fluazinam in/on apple were above the LLMV 

(LLMV = 0.01 ppm). The apple dataset was large (42 samples). The result from the 

approximate Shapiro-Francia test statistic (Figure II-2) indicated that the assumption of 

lognormality should be rejected. Visual inspection of the lognormal probability plot (Figure II-1) 

provided in the spreadsheet confirmed that the dataset is not lognormal. Using the tolerance 

spreadsheet, the recommended tolerance is 1.5 ppm for apple.
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 43 of 54

Table II-1. Fluazinam Residues in/on Apples Following Nine to Twelve Foliar Applications of 

Fluazinam (FlC) at Rates Totaling ~4.5 lb ai/A/season.

Regulator: EPA EPA

Chemical: Fluazinam Fluazinam

Crop: Apple Apple

PHI: 28-32 Days 28-29 Days

Total App. Rate: 3.97-5.40 lb ai/A 4.44-4.77 lb ai/A

Submitter: ISK Biosciences Corporation ISK Biosciences Corporation

MRID Citation: MRIDs 47756607, 47756608, 47756610, 

and 47756611

MRID 47756609

Residues of Fluazinam (ppm) 1

0.050 0.160

0.030 0.160

0.050 0.160

0.03 0.160

0.05 0.030

0.060 0.020

0.030 0.090

0.040 0.150

0.010 0.150

0.010 0.120

0.010 0.150

0.010 0.120

0.020 1.680

0.040 1.390

0.020 0.050

0.040 0.020

0.080 0.170

0.080 0.090

0.020 1.310

0.030 1.490

0.150

0.130

0.050

0.300

0.120

0.170

1 Residue values <LLMV (0.01 ppm) are listed in bold.
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 44 of 54

Figure II-1. Lognormal probability plot of fluazinam field trial data for apple.

Lognormal Probability Plot

0.1 1 2 5 10 20 30 50 70 80 90 95 98 99 99.9

2.0000

1.0000

0.5000

0.2500

0.1250

0.0625

0.0313

0.0156

0.0078

y = 1.3151x - 2.6003

R

2

 = 0.932

Percentiles

Concentrations

EPA Fluazinam Apples 28 Days

Figure II-2. Tolerance spreadsheet summary of fluazinam field trial data for apple.

Regulator: EPA

Chemical: Fluazinam

Crop: Apples

P HI: 28 Days

App. Rate:

Submitter:

n: 42

m in: 0.01

m ax: 1.68

median: 0.07

a verage: 0.21

95th Percentile 9 9th Percentile 99.9th Percentile

1.0 1.2 1.6

(1.1) ( 1.5) (--)

0 .70 1.7 5.0

(1.3) ( 4.0) (--)

0.30

1.5

0.35

0.9320

0.05 >= p-value > 0.01 : Reject lognormality assumption

Approximate 

Shapiro-Francia

Normality Test 

EU Method I

Normal

U CLMedian95th

95/99 Rule

EU Method II

Distribution-Free

M ean+3SD
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 45 of 54

Bulb Onions (Subgroup 3-07A)

The dataset used to establish a tolerance for fluazinam on the bulb onion subgroup consisted of 

field trial data for bulb onions representing application rates of 3.11-3.17 lb ai/A (6 applications 

at ~0.52 lb ai/A/application) with PHIs of 6-8 days. As specified by the SOP, the trial 

application rates and PHIs are within 25% of the maximum label application rate and minimum 

label PHI, respectively. The residue values used to calculate the tolerance for bulb onion are 

provided in Table II-2.

As 7 of the 18 field trial sample results for bulb onion were <LOQ, maximum likelihood 

estimation (MLE) procedures were used to impute the censored values for onions. The censored 

dataset for onions, which consisted of 18 samples, was then entered into the tolerance 

spreadsheet. Visual inspection of the lognormal probability plot (Figure II-3) and the results 

from the approximate Shapiro-Francia test statistic (Figure II-4) indicate that the dataset is 

reasonably lognormal. 

The recommended tolerance is 0.20 ppm for bulb onion, which is the representative crop for the 

bulb onion subgroup 3-07A. 

Table II-2. Fluazinam Residues in/on Onions Following Six Foliar Applications of Fluazinam (FlC) at 

Rates Totaling ~3.12 lb ai/A/season.

Regulator: EPA

Chemical: Fluazinam

Crop: Bulb Onion (MLE)

PHI: 6-8 days 

App. Rate: 3.11-3.17 lb ai/A

Submitter: IR-4

MRID Citation: MRID 47631001

Residues (ppm)

1

0.002 0.015

0.003 0.016

0.004 0.021

0.005 0.031

0.006 0.033

0.007 0.035

0.009 0.045

0.013 0.095

0.013 0.101

1

 Residue values <LLMV (0.01 ppm) are listed in bold.
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 46 of 54

Figure II-3. Lognormal probability plot of fluazinam field trial data for bulb onion.

Lognormal Probability Plot

0.1 1 2 5 10 20 30 50 70 80 90 95 98 99 99.9

1.0000

0.5000

0.2500

0.1250

0.0625

0.0313

0.0156

0.0078

0.0039

0.0020

y = 1.1368x - 4.2304

R

2

 = 0.9858

Percentiles

Concentrations

EPA Fluazinam Bulb Onion (MLE) 6-8 days 3.11-3.17 lb ai/A IR-4

Figure II-4. Tolerance spreadsheet summary of fluazinam field trial data for bulb onion.

Regulator: EPA

Chemical: Fluazinam

Crop: Bulb Onion (MLE)

PHI: 6-8 days 

App. Rate: 3.11-3.17 lb ai/A

Submitter: IR-4

n: 18

min: 0.00

max: 0.10

median: 0.01

average: 0.03

95th Percentile 99th Percentile 99.9th Percentile

0.08 0.10 0.15

(0.10) (0.15) (--)

0.09 0.20 0.45

(0.25) (0.60) (--)

0.07

0.15

0.08

0.9858

p-value > 0.05 : Do not reject lognormality assumption

Approximate 

Shapiro-Francia 

Normality Test 

EU Method I

Normal

UCLMedian95th

95/99 Rule

EU Method II

Distribution-Free

Mean+3SD
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 47 of 54

Bushberry subgroup (13-07B)

Based on previously reviewed blueberry data (PP# 6E7137; D335640, W. Drew, 8/22/07), a 7.0

ppm tolerance was established on the Bushberry subgroup 13B and several related bushberry

crops. To assess IR-4’s request to lower the bushberry tolerance, HED has reexamined the 

original blueberry residue data supporting the tolerance (Table II-3). Only the fluazinam residue 

data were included, as fluazinam per se is the residue of concern for tolerance assessment. 

The data were entered into the tolerance spreadsheet. The results from the approximate ShapiroFrancia test statistic (Figure II-6) indicated that the assumption of lognormality should not be 

rejected. Therefore, the recommended tolerance for the Bushberry subgroup 13-07B is 7.0 ppm.

Table II-3. Fluazinam Residues in/on Blueberries Following Six Foliar Applications of Fluazinam (FlC) 

at Rates Totaling ~3.12 lb ai/A/season.

Regulator: EPA

Chemical: Fluazinam

Crop: Blueberry

PHI: 23-32 Days

App. Rate: 3.8-4.1 lb ai/A

Submitter: IR-4

MRID Citation: MRID 46986701

Residues (ppm)

1

0.064 0.64

0.070 0.68

0.074 0.70

0.12 1.0

0.13 1.2

0.16 1.2

0.17 1.5

0.42 1.6

0.45 1.6

0.49 1.7

0.50 2.0

0.55
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 48 of 54

Figure II-5. Lognormal probability plot of fluazinam field trial data for blueberry.

Lognormal Probability Plot

0.1 1 2 5 10 20 30 50 70 80 90 95 98 99 99.9

2.0000

1.0000

0.5000

0.2500

0.1250

0.0625

y = 1.1139x - 0.7696

R

2

 = 0.9251

Percentiles

Concentrations

EPA Fluazinam Blueberry 23-32 Days 3.8-4.1 lb ai/A IR-4
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 49 of 54

Figure II-6. Tolerance spreadsheet summary of fluazinam field trial data for blueberry.

Regulator: EPA

Chemical: Fluazinam

Crop: Blueberry

PHI: 23-32 Days

App. Rate: 3.8-4.1 lb ai/A

Submitter: IR-4

n: 23

min: 0.06

max: 2.00

median: 0.55

average: 0.74

95th Percentile 99th Percentile 99.9th Percentile

1.8 2.5 3.0

(2.5) (3.0) (--)

3.0 7.0 15

(7.0) (17) (--)

2.5

3.0

3.0

0.9251

p-value > 0.05 : Do not reject lognormality assumption

Approximate 

Shapiro-Francia 

Normality Test 

EU Method I

Normal

UCLMedian95th

95/99 Rule

EU Method II

Distribution-Free

Mean+3SD

Carrot

The dataset used to establish a tolerance for fluazinam on carrot consisted of field trial data 

representing application rates of 2.04-3.03 lb ai/A (4-5 applications at 0.492-0.786 lb 

ai/A/application) with PHIs of 6-8 days. Each field trial consisted of two treatment plots 

(Treatments 2 and 3). Both plots received treatments in similar rates and volumes; however, 

Treatment 2 was irrigated within 2 hours of each application, and Treatment 3 received irrigation 

after 24 hours of each application. As specified by the SOP, the trial application rates and PHIs 

are within 25% of the maximum label application rate and minimum label PHI, respectively. 

The residue values used to calculate the tolerance for carrot are provided in Table II-4.

All but 4 of the 52 field trial sample results for fluazinam in/on carrot were above the LLMV 

(LLMV = 0.02 ppm). The carrot dataset was large (52 samples). Visual inspection of the 

lognormal probability plot (Figure II-7) and the results from the approximate Shapiro-Francia test 

statistic (Figure II-8) indicated that the carrot dataset was reasonably lognormal. Using the 

tolerance spreadsheet, the recommended tolerance is 0.7 ppm for carrot.
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 50 of 54

Table II-4. Fluazinam Residues in/on Carrots Following Four to Five Foliar Applications of 

Fluazinam (FlC) at Rates Totaling ~2.09 lb ai/A/season.

Regulator: EPA EPA

Chemical: Fluazinam Fluazinam

Crop: Carrot (Treatment 2; irrigated w/in 2 hours 

of each application)

Carrot (Treatment 3; irrigated after 24 

hours of each application)

PHI: 6-8 Days 6-8 Days

Total App. Rate: 2.04-2.94 lb ai/A 2.04-3.03 lb ai/A

Submitter: IR-4 IR-4

MRID Citation: MRID 47756601 MRID 47756601

Residues of Fluazinam (ppm) 1

0.040 0.050

0.060 0.060

0.340 0.240

0.390 0.280

0.020 0.020

0.020 0.020

0.120 0.030

0.120 0.040

0.120 0.100

0.140 0.110

0.050 0.170

0.060 0.190

0.110 0.410

0.120 0.450

0.070 0.050

0.190 0.070

0.460 0.160

0.560 0.250

0.100 0.090

0.100 0.090

0.090 0.080

0.110 0.090

0.220 0.020

0.230 0.020

0.080 0.040

0.090 0.050

1 Residue values <LLMV (0.02 ppm) are listed in bold.
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 51 of 54

Figure II-7. Lognormal probability plot of fluazinam field trial data for carrot.

Lognormal Probability Plot

0.1 1 2 5 10 20 30 50 70 80 90 95 98 99 99.9

1.0000

0.5000

0.2500

0.1250

0.0625

0.0313

0.0156

y = 0.9014x - 2.3559

R

2 = 0.9756

Percentiles

Concentrations

EPA Fluazinam Carrot (combined irrigation data) 6-8 Days 2.04-3.03 lb ai/A IR-4

Figure II-8. Tolerance spreadsheet summary of fluazinam field trial data for carrot.

Regulator: EPA

Chemical: Fluazinam

Crop: Carrot (combined irrigation data)

PHI: 6-8 Days

App. Rate: 2.04-3.03 lb ai/A

Submitter: IR-4

n: 52

min: 0.02

max: 0.56

median: 0.10

average: 0.14

95th Percentile 99th Percentile 99.9th Percentile

0.35 0.45 0.60

(0.45) (0.60) (--)

0.45 0.80 1.6

(0.70) (1.3) (--)

0.40

0.60

0.50

0.9756

p-value > 0.05 : Do not reject lognormality assumption

Approximate 

Shapiro-Francia 

Normality Test 

EU Method I

Normal

UCLMedian95th

95/99 Rule

EU Method II

Distribution-Free

Mean+3SD
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 52 of 54

Head Lettuce

The dataset used to assess a tolerance for fluazinam residues on head lettuce consisted of field 

trial data representing application rates of 0.952-1.02 lb ai/A with PHIs of 46-52 days. As 

specified by the SOP, the field trial application rates and PHIs are within 25% of the maximum 

label application rate and minimum label PHI, respectively. Because all but one of the residue 

values for head lettuce were <LOQ (<0.01 ppm), the tolerance spreadsheet could not be used to 

calculate a possible tolerance (Table II-5). Therefore, the maximum residue value (0.021 ppm) 

was used to determine the tolerance. 

Table II-5. Fluazinam Residues in/on Head Lettuce Following a Broadcast Foliar Application of 

Fluazinam (FlC) at a Rate of ~0.99 lb ai/A/season.

Regulator: EPA

Chemical: Fluazinam

Crop: Head Lettuce

PHI: 46-52 days 

App. Rate: 0.952-1.02 lb ai/A

Submitter: IR-4

MRID Citation: MRID 47631002

Residues (ppm)

1

0.01 0.01

0.01 0.01

0.01 0.01

0.01 0.01

0.01 0.01

0.01 0.01

0.01 0.021

1

 Residue values <LLMV (0.01 ppm) are listed in bold.

Leaf Lettuce

The dataset used to assess a tolerance for fluazinam residues on leaf lettuce consisted of field 

trial data representing application rates of 0.974-1.05 lb ai/A with PHIs of 20-32 days. As 

specified in the SOP, the field trial application rates and PHIs are within 25% of the maximum 

label application rate and minimum label PHI, respectively. The residue values used to calculate 

the tolerance are provided in Table II-6. 

The leaf lettuce dataset, which is relatively small (14 samples), was entered into the tolerance 

spreadsheet. Field trial sample results were above the LLMV (0.01 ppm) for 12 of 14 samples. 

Visual inspection of the lognormal probability plot (Figure II-9) and the result from the 

approximate Shapiro-Francia test statistic (Figure II-10) indicated that the assumption of 

lognormality should be rejected. 

Using the tolerance spreadsheet, the recommended value is 2.0 ppm for leaf lettuce. 
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 53 of 54

Table II-6. Fluazinam Residues in/on Leaf Lettuce Following a Broadcast Foliar Application of 

Fluazinam (FlC) at a Rate of ~0.99 lb ai/A/season.

Regulator: EPA

Chemical: Fluazinam

Crop: Leaf Lettuce

PHI: 20-32 days

App. Rate: 0.974-1.05 lb ai/A

Submitter: IR-4

MRID Citation: MRID 47631002

Residues (ppm)

1

0.01 0.021

0.01 0.022

0.011 0.038

0.017 0.150

0.019 0.159

0.020 1.45

0.020 1.69

1

 Residue values <LLMV (0.01 ppm) are listed in bold.

Figure II-9. Lognormal probability plot of fluazinam field trial data for leaf lettuce.

Lognormal Probability Plot

0.1 1 2 5 10 20 30 50 70 80 90 95 98 99 99.9

2.0000

1.0000

0.5000

0.2500

0.1250

0.0625

0.0313

0.0156

0.0078

y = 1.6054x - 3.098

R

2

 = 0.7821

Percentiles

Concentrations

EPA Fluazinam Leaf Lettuce 20-32 days 0.974-1.05 lb ai/A IR-4
Fluazinam Summary of Analytical Chemistry and Residue Data DP#: 360840

Page 54 of 54

Figure II-10. Tolerance spreadsheet summary of fluazinam field trial data for leaf lettuce.

Regulator: EPA

Chemical: Fluazinam

Crop: Leaf Lettuce

PHI: 20-32 days

App. Rate: 0.974-1.05 lb ai/A

Submitter: IR-4

n: 14

min: 0.01

max: 1.69

median: 0.02

average: 0.26

95th Percentile 99th Percentile 99.9th Percentile

1.2 1.6 2.0

(1.8) (2.5) (--)

0.80 3.0 10

(4.5) (25) (--)

0.35

2.0

0.15

0.7821

p-value <= 0.01: Reject lognormality assumption

Approximate 

Shapiro-Francia 

Normality Test 

EU Method I

Normal

UCLMedian95th

95/99 Rule

EU Method II

Distribution-Free

Mean+3SD