Acequinocyl Summary of Analytical Chemistry and Residue Data

UNITED STATES ENVIRONMENTAL PROTECTION AGENCY

 

MEMORANDUM

Date: 30-NOV-2011

SUBJECT: Acequinocyl. Petition for 

Shelled Beans; Cowpea Forage; Caneberry Subgroup 13

9A; Cucumber, Cherry; Low

Vine Climbing, Except Fuzzy Kiwifruit, Subgroup 13

Analytical Chemistry and Residue Data

PC Code: 006329

Decision No.: 448205

Petition No.: 1E7864

Risk Assessment Type: NA

TXR No.: NA

MRID Nos.: 484629-01 thru -05

FROM: Sarah J. Levy, Chemist

Risk Assessment Branch 1 (RAB1)

Health Effects Division (HED

THROUGH: George F. Kramer, Ph.D., 

RAB1/HED (7509P

TO: Barbara Madden, RM

Registration Division (RD; 7505P)

Executive Summary

Acequinocyl is a quinoline-type miticide registered for use 

agricultural commodities (RACs)

Acequinocyl is currently registered to Arysta Lifescience North America Corporation as a 15% 

suspension-concentrate (SC) formulation. 

were a joint-review with Canada.

Under PP#1E7864, the Interregional Research Project No.4 (IR

Experiment Station of TX, CA, OR, PA, GA, NM, OK, TN, UT, MI, FL, and AZ

for the establishment of tolerances for combined residues of the insecticide acequinocyl, 2

(acetyloxy)-3-dodecyl-1,4-naphthalenedione, and its metabolite, 2

naphthoquinone (acequinocyl-OH)

Summary of Analytical Chemistry and Residue Data

Page 1 of 30

UNITED STATES ENVIRONMENTAL PROTECTION AGENCY

WASHINGTON, D.C. 20460 

OFFICE OF CHEMICAL SAFETY AND

 POLLUTION PREVENTION

etition for Use on Succulent Soybean Vegetable; Succulent 

Shelled Beans; Cowpea Forage; Caneberry Subgroup 13-07A; Melon Subgroup 

9A; Cucumber, Cherry; Low-Growing Berry Subgroup 13-07G; and Small Fruit 

Vine Climbing, Except Fuzzy Kiwifruit, Subgroup 13-07F. Summary of 

Analytical Chemistry and Residue Data. 

DP Barcode: D389989

Registration No.: 66330-38

Regulatory Action: Section 3

Case No.: 7621

CAS No.: 57960-19-7

5 40 CFR: §180.599

Chemist

Risk Assessment Branch 1 (RAB1)

Health Effects Division (HED; 7509P)

George F. Kramer, Ph.D., Senior Chemist

7509P)

Barbara Madden, RM Team 05

Registration Division (RD; 7505P)

type miticide registered for use in the U.S. on a number of raw 

agricultural commodities (RACs) for the control of various phytophagous mite species

Acequinocyl is currently registered to Arysta Lifescience North America Corporation as a 15% 

concentrate (SC) formulation. Note that the cucumber and caneberry field trial data 

review with Canada.

Interregional Research Project No.4 (IR-4), on behalf of the Agricultural 

TX, CA, OR, PA, GA, NM, OK, TN, UT, MI, FL, and AZ

he establishment of tolerances for combined residues of the insecticide acequinocyl, 2

naphthalenedione, and its metabolite, 2-dodecyl-3-hydroxy

OH), expressed as acequinocyl equivalents in/on the f

DP#: 389989

UNITED STATES ENVIRONMENTAL PROTECTION AGENCY

OFFICE OF CHEMICAL SAFETY AND

POLLUTION PREVENTION

Succulent Soybean Vegetable; Succulent 

07A; Melon Subgroup 

07G; and Small Fruit 

Summary of 

number of raw 

for the control of various phytophagous mite species. 

Acequinocyl is currently registered to Arysta Lifescience North America Corporation as a 15% 

er and caneberry field trial data 

, on behalf of the Agricultural 

TX, CA, OR, PA, GA, NM, OK, TN, UT, MI, FL, and AZ, is requesting 

he establishment of tolerances for combined residues of the insecticide acequinocyl, 2 -

hydroxy-1,4-

in/on the following 
Acequinocyl Summary of Analytical Chemistry and Residue Data DP#: 389989

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commodities:

 Soybean, vegetable, succulent ..................................................................0.25 ppm

 Low growing berry subgroup 13-07G ......................................................0.4 ppm

 Small fruit vine climbing subgroup 13-07F, except fuzzy kiwifruit ........1.6 ppm

 Bean, succulent shelled.............................................................................0.15 ppm

 Cowpea, forage .........................................................................................9.0 ppm

 Caneberry subgroup 13-07A.....................................................................4.5 ppm

 Melon subgroup 9A ..................................................................................0.06 ppm

 Cucumber..................................................................................................0.15 ppm

 Cherry .......................................................................................................0.8 ppm

No new data were submitted to support tolerances on succulent soybean vegetables, low-growing 

berry 13-07G crop subgroup, or small fruit vine climbing subgroup 13-07F, except fuzzy

kiwifruit. The petitioner has requested that existing tolerances be expanded to their respective 

crops or crop groups.

The end-use product proposed for use on the aforementioned proposed crops is KanemiteTM 15 

SC Miticide, a 1.25 lb/gal soluble concentrate (SC) formulation (alternate brand names: 

ShuttleTM 15 SC Miticide, and ShuttleTM O Miticide). Up to two foliar, postemergence, ground

applications are proposed for a maximum seasonal rate of 0.6 lb ai/A, with a 1-day preharvest 

interval (PHI), except for succulent shelled beans and cherries for which a 7-day PHI is 

proposed.

Tolerances are currently established under 40 CFR §180.599(a) for the combined residues of 

acequinocyl and its metabolite, 2-dodecyl-3-hydroxy-1,4-naphthoquinone, expressed as 

acequinocyl equivalents, in/on a number of plant and livestock commodities. Tolerances for 

plant commodities range from 0.02 ppm (tree nuts and pistachios) to 30 ppm (citrus oil), and 

tolerances for livestock commodities are established at 0.02 ppm in the fat and liver of cattle, 

goat, horse, and sheep.

The nature of acequinocyl residues in apples, oranges, and eggplants is understood based on the 

previously reviewed metabolism studies. In these crops, the metabolism of acequinocyl involves 

the loss of the acetyloxy moiety to form acequinocyl-OH, the opening of the quinone ring to 

form AKM-18, and the subsequent degradation of the quinone ring to yield polar metabolites 

that degrade to phthalic acid. For purposes of risk assessment and the tolerance expression, HED

has determined that the residues of concern in these commodities include parent and 

acequinocyl-OH (Memo, S. Levy, 07-JAN-2004; DP# 297872). These data are considered 

sufficient for the currently requested crops.

There are adequate residue analytical methods for enforcing tolerances for acequinocyl residues 

of concern in/on the proposed/registered commodities. These methods include two highperformance liquid chromatography methods with tandem mass-spectroscopy detection 

(HPLC/MS/MS) for determining residues in/on plant commodities (Morse Methods Meth-135

and #Meth-133, revision #3). For each of these methods, residues are extracted with hexane or 

acetonitrile (ACN)/water and cleaned up by solvent partitioning, gel-permeation chromatography 

(GPC) and/or silica-gel solid-phase extraction (SPE). In the current field trials, residues of 

acequinocyl and acequinocyl-OH were determined using a modified version of Morse Method 

#Meth-133, revision #3. The method limit of quantitation (LOQ; based on the lowest level of 
Acequinocyl Summary of Analytical Chemistry and Residue Data DP#: 389989

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method validation (LLMV)) for succulent shelled beans was 0.02 ppm for each analyte. The 

LOQ (based on the LLMV) for cantaloupe was 0.015 ppm for acequinocyl and 0.01 ppm for 

acequinocyl-OH. For cherries, cucumbers, and caneberries, the LOQ (based on the LLMV) was 

0.01 for each analyte. The method was adequately validated in conjunction with the analysis of 

field trial samples. 

Based on the potential dietary exposure of livestock to acequinocyl residues from the current and 

proposed uses, the dietary burden was re-evaluated. The re-evaluated dietary burden indicates

that the currently established tolerance level of 0.02 ppm for residues in cattle, goat, horse, and 

sheep fat are appropriate. The established 0.02-ppm residue level in cattle, goat, horse, and 

sheep liver is appropriate; however, the commodity definition should be changed to “meat 

byproducts” rather than “liver.” With the establishment of the cattle, goat, horse, and sheep 

tolerance in meat byproducts, RD should remove the tolerance (40 CFR §180.599) for liver. 

Furthermore, the meat byproducts tolerance of 0.02 ppm is adequate to cover residues in the 

kidney of cattle, goats, horses, and sheep. A revised Section F should be submitted.

The data requirements for multiresidue (MRM) methods are fulfilled. Certain MRM protocols 

resulted in acceptable recoveries. The MRM testing data have been forwarded to the U.S. Food 

and Drug Administration (FDA) for further evaluation (Memo, S. Levy, 18-FEB-2004; DP#

298917).

The submitted concurrent storage stability data for the subject crops are adequate to support the 

storage intervals and conditions incurred by the field trial studies. 

IR-4 submitted adequate field trial data in support of the proposed uses on succulent shelled 

beans, caneberry, cantaloupe, cherry, and cucumber. The field trials reflect the proposed use 

patterns and an adequate number of field trials were conducted in major crop growing regions. 

The submitted field trial data reflect applications made without the use of a spray adjuvant. A 

revised Section B should be submitted prohibiting the addition of adjuvants to the spray 

solution. The Organization for Economic Co-operation and Development (OECD) maximum 

residue limit (MRL) Calculator was used to determine the appropriate tolerance levels. The field 

trial data will support tolerances of: 0.30 ppm for residues in/on bean, succulent shelled; 6.0 

ppm for residues in/on cowpea, forage; 18 ppm for residues in/on cowpea, hay; 4.0 ppm for

residues in/on caneberry subgroup 13-07A; 0.15 ppm for residues in/on melon subgroup 9A; 1.0 

ppm for residues in/on cherry, tart; 0.50 ppm for residues in/on cherry, sweet; and 0.15 ppm for 

residues in/on cucumber. A revised Section F should be submitted. 

No new data were submitted to support tolerances on succulent soybean vegetables, low-growing 

berry 13-07G crop subgroup, or small fruit climbing vine subgroup 13-07F, except fuzzy

kiwifruit. However, existing established tolerances in 40 CFR §180.599 should be extended to 

support these crop group tolerances. HED recommends that that the tolerance for residues in/on 

edible-podded beans should be extended to soybean, vegetable, succulent; the tolerance for 

residues in/on strawberries should be extended to the low-growing berry 13-07G subgroup; and 

the tolerance for residues in/on grapes should be extended to small fruit vine climbing subgroup 

13-07F, except fuzzy kiwifruit (See Table 10 for details).

There are no processed food/feed items associated with the proposed uses. Therefore, data 

requirements for this guideline are not relevant to this tolerance petition.
Acequinocyl Summary of Analytical Chemistry and Residue Data DP#: 389989

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The proposed uses under this petition include the following typically rotated crops: succulent 

soybeans, berries (subgroup 13-07G), succulent shelled beans, cowpea forage, cucumbers, and 

melons (subgroup 9A). An adequate confined rotational crop study was submitted and reviewed 

with a previous petition. The available data support a 30-day plantback interval (PBI) for all 

non-labeled crops, which is reflected on the proposed label.

Regulatory Recommendations and Residue Chemistry Deficiencies

Pending submission of revised Sections B (see requirements under Directions for Use) and F (see 

requirements under Proposed Tolerances) there are no residue chemistry issues that would 

preclude granting a permanent registration for the requested uses of acequinocyl or establishment 

of tolerances for residues of acequinocyl and acequinocyl-OH as follows: “tolerances are 

established for residues of acequinocyl, including its metabolites and degradates, in or on the 

commodities in the table below. Compliance with the tolerance levels specified below is to be 

determined by measuring only the sum of acequinocyl [2-(acetyloxy)-3-dodecyl-1,4-

naphthalenedione] and its metabolite, 2-dodecyl-3-hydroxy-1,4-naphthoquinone, calculated as 

the stoichiometric equivalent of acequinocyl, in or on the commodity.”

Soybean, vegetable, succulent ....................................................... 0.25 ppm

Low growing berry subgroup 13-07G1 .............................................. 0.50 ppm

Small fruit vine climbing subgroup 13-07F, except fuzzy kiwifruit1... 1.6 ppm

Bean, succulent shelled................................................................................. 0.30 ppm

Cowpea, forage........................................................................... 6.0 ppm

Cowpea, hay................................................................................. 18 ppm

Caneberry subgroup 13-07A............................................................ 4.0 ppm

Melon subgroup 9A........................................................................ 0.15 ppm

Cucumber...................................................................................... 0.15 ppm

Cherry, tart................................................................................. 1.0 ppm

Cherry, sweet.............................................................................. 0.50 ppm

Meat byproducts of cattle, goat, horse and sheep1 ........................... 0.02 ppm

1

 Note to RD: With the establishment of these tolerances, the following tolerances should be removed: strawberry; 

grape; and liver of cattle, goat, horse, and sheep.

A human-health risk assessment is forthcoming (DP# 389519).

860.1200 Directions for Use

 The submitted field trial data reflect applications made without the use of a spray

adjuvant. A revised Section B should be submitted incorporating an adjuvant–use 

restriction.

860.1550 Proposed Tolerances

 A revised Section F is required to amend the tolerances as specified in Table 10, as well 

as the tolerance expression (see Conclusions section under Table 10 for details).
Acequinocyl Summary of Analytical Chemistry and Residue Data DP#: 389989

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Background

The chemical structure and nomenclature of acequinocyl and its regulated metabolite are 

presented in Table 1, and the physicochemical properties of acequinocyl are presented in Table 

2. 

Table 1. Nomenclature of Test Compound and Metabolites.

Compound

O

O

CH2(CH2)

10CH3

OCOCH3

Common name Acequinocyl

Company experimental names TM-41301 or AKD-2023

IUPAC name 3-dodecyl-1,4-dihydro-1,4-dioxo-2-naphthyl acetate

CAS name 2-(acetyloxy)-3-dodecyl-1,4-naphthalenedione

CAS # 57960-19-7

End-use products/EP KanemiteTM 15 SC (1.25 lb ai/gal; EPA Reg. No. 66330-38)

Compound O

O

CH2(CH2)

10CH3

OH

Common name Acequinocyl-OH

Company experimental names R1

IUPAC name 2-dodecyl-3-hydroxy-1,4-napthoquinone

CAS name 2-dodecyl-3-hydroxy-1,4-naphthalenedione

CAS # 57960-31-3

Table 2. Physicochemical Properties.

Parameter Value Reference (MRID)

Melting point 59.6 C 45434906

pH 6.94 45434904

Density 1.13 g/cm345434904

Water solubility (20°C) 6.69 μg/L 45434906

Solvent solubility (mg/L at 20°C) 1,2-dichloroethane: >250

acetone: >250

ethyl acetate: >250

xylene: >250

methanol: 6.1

n-heptane: 36

n-octanol: 29.2

45434904

Vapor pressure at 25°C 1.69 x 10-9pascals 45434905

Dissociation constant (pKa) no measurable pKa 45434905

Octanol/water partition coefficient 

Log(KOW)

>6.2 45434906

UV/visible absorption spectrum

(max, nm)

neutral pH: 242, 248, 262, 270, 335

acid pH: 242, 248, 265, 270, 330

basic pH: 232, 245, 255, 275, 362

45434905
Acequinocyl Summary of Analytical Chemistry and Residue Data DP#: 389989

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860.1200 Directions for Use

The petitioner provided a draft label for KanemiteTM 15 SC Miticide (EPA Reg. No. 66330-38), 

a 1.25 lb/gal SC formulation of acequinocyl. This acequinocyl formulation is currently 

registered for use on several fruit and nut crops, fruiting vegetables, okra, edible-podded beans,

and hops. The proposed uses are summarized below in Table 3.

Table 3. Summary of Proposed Directions for Use of Acequinocyl.

Applic. Timing, 

Type, and 

Equip.

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

Bean, succulent shelled

Postemergence,

foliar;

Ground only

1.25 lb/gal

SC

[66330-38]

0.3 2 0.6 7

Minimum spray volume 

of 30 gal/A; minimum 

RTI of 14 days. Do not 

allow grazing on cowpea 

forage within 7 days of 

last treatment.

Caneberry subgroup 13-07A

Postemergence,

foliar;

Ground only

1.25 lb/gal 

SC

[66330-38]

0.3 2 0.6 1

Minimum spray volume 

of 50 gal/A; minimum 

RTI of 21 days.

Melon subgroup 9A

Postemergence,

foliar;

Ground only

1.25 lb/gal 

SC

[66330-38]

0.3 2 0.6 1

Minimum spray volume 

of 30 gal/A; minimum 

RTI of 21 days.

Cucumber

Postemergence, 

foliar;

Ground only

1.25 lb/gal 

SC

[66330-38]

0.3 2 0.6 1

Minimum spray volume 

of 100 gal/A; minimum 

RTI of 21 days. The use 

of an adjuvant or 

surfactant is prohibited.

Cherry

Postemergence, 

foliar;

Ground only

1.25 lb/gal 

SC

[66330-38]

0.3 2 0.6 7

Minimum spray volume 

of 40 gal/A; for optimal 

control, use a minimum 

of 150 gal/A; minimum 

RTI of 14 days. Do not 

use in alternate row 

middle applications.

1

 RTI = retreatment interval.

General label restrictions include: (i) do not apply through any type of irrigation system; (ii) do 

not apply by air; (iii) do not apply within 75 feet of aquatic areas; and (iv) not for indoor 

residential use. The product may be combined with most commonly used pesticides with the 

exception of strongly alkaline material, which can reduce activity; combination with Phos-ethyl 

(fosetyl) is prohibited. Broad-spectrum insect control may be obtained by tank-mixing the SC 

acequinocyl product with other miticide/insecticide products; a spray mix compatibility and 

phytotoxicity trial under local conditions should first be conducted. 
Acequinocyl Summary of Analytical Chemistry and Residue Data DP#: 389989

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Rotational crop restrictions are as follows: food and feed crops not listed on the proposed label 

must not be planted within 30 days of the last KanemiteTM 15 SC application.

Conclusions: The proposed use directions are adequate to allow for evaluation of the submitted 

residue data relative to the proposed uses. The proposed uses are supported by the submitted 

field trial data.

Furthermore, the submitted field trial data reflect applications made without the use of a spray

adjuvant. A revised Section B should be submitted incorporating an adjuvant–use 

restriction.

An adequate confined rotational crop study was previously submitted, reflecting the maximum 

proposed use pattern for rotated crops. The available data support a 30-day PBI for all nonlabeled crops, which is reflected on the proposed label.

860.1300 Nature of the Residue – Plants/Livestock

The qualitative nature of acequinocyl residues in fruit and nut crops is understood based on the 

available apple, orange, and eggplant metabolism studies (Memo, S. Levy, 10-MAR-2004; DP# 

284757). Residues in/on both the fruit and foliage were characterized in these metabolism 

studies. The data indicate that the metabolism of acequinocyl in these crops involves the loss of 

the acetyloxy moiety to form acequinocyl-OH, opening of the quinone ring to form AKM-18, 

and subsequent degradation of the quinone ring to yield polar metabolites that degrade to 

phthalic acid. 

Based on the structural similarity of acequinocyl-OH to parent and the presence of acequinocylOH at quantifiable levels in crops, the HED Metabolism Assessment Review Committee 

(MARC) concluded that parent and acequinocyl-OH are the residues of concern for risk 

assessment and tolerance expression in apples, oranges, and eggplant commodities (Memo, S. 

Levy, 07-JAN-2004; DP# 297872). For purposes of this petition, HED is willing to translate 

these results to caneberries, cantaloupe, cherry, and cucumber as these are fruit crops and 

succulent shelled beans is a low-consumption food item. However, if in the future, the petitioner 

requests new uses where apple, orange, and eggplant metabolism data cannot be translated, then 

HED may ask for additional plant metabolism data.

The qualitative nature of acequinocyl residues in ruminants is understood based on an adequate 

goat metabolism study (Memo, S. Levy, 10-MAR-2004; DP# 284757). The metabolism of 

acequinocyl in goats appears to involve the loss of the acetyloxyl moiety to form acequinocylOH and partial cleavage of the dodecyl side chain to form AKM-15. Opening and degradation 

of the quinone ring was also evidenced by the presence of AKM-18 and phthalic acid. The 

MARC concluded that for tolerance expression, the residues of concern in livestock commodities 

include parent and acequinocyl-OH. For risk assessment purposes, the residues of concern in 

livestock commodities are parent and acequinocyl-OH (for liver and kidney, metabolite AKM-15 

is to be included as well (Memo, S. Levy, et al., 07-JAN-2004; DP# 297872). 

Metabolism data on poultry are not required at the present time as none of the proposed or 

existing uses of acequinocyl are on crops having regulated poultry feedstuffs.
Acequinocyl Summary of Analytical Chemistry and Residue Data DP#: 389989

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860.1340 Residue Analytical Methods

Enforcement methods: Adequate analytical methods are available for enforcing acequinocyl 

tolerances in/on the proposed/registered plant commodities (Memo, D. Soderberg 23-MAY2006; DP# 321753; Memo, S. Levy, 25-JUN-2008; DP#s 351336 & 353313). These methods 

include two HPLC/MS/MS methods for determining acequinocyl and acequinocyl-OH residues 

in fruit crops (Morse Method #Meth-133, revision #3) and nut crops (Morse Method #Meth135). The three methods were forwarded by HED to Biological and Economical Analysis 

Division’s (BEAD’s) Analytical Chemistry Branch (ACB) for a petition method validation 

(PMV). In lieu of a PMV, ACB completed a desk audit (Memo, P. Golden, 04-APR-2006; 

ACB# B04-13) in which ACB recommended that the petitioner revise methods # Meth-133, 

Revision #3 (including the modification for orange oil), # Meth-135, and # Meth-139 Revision

#2 to address deficiencies. The petitioner adequately addressed the modifications requested by 

ACB (Memo, P. Golden, 04-APR-2006; ACB# B04-13). Methods #Meth-135, Revision #3, 

#Meth-133, Revision #4, and #Meth-139, Revision #3 are suitable enforcement methods for the 

subject crop and livestock matrices and no additional data concerning these methods are 

necessary (Memo, S. Levy, 25-AUG-2010; DP# 380302).

Data-gathering methods: Samples of crop commodities that were collected from the magnitude 

of the residue studies were analyzed for residues of acequinocyl and acequinocyl-OH using 

modifications of the enforcement methods. Samples from all submitted field trials were 

analyzed using a modified version of Method Meth-133. A summary is given below.

Briefly, 10-g samples were extracted with ACN. Extra water was added to insure that a 

minimum amount of water was available for adequate analyte extraction. Following extraction, 

the water was salted out, and an aliquot of the resulting ACN phase was extracted with hexane to 

separate the analytes from the undesirable ACN-soluble co-extracted materials. A final 

purification, incorporating silica SPE cartridge cleanup, was conducted. The purified extract was 

concentrated and then submitted to HPLC/MS/MS analysis. 

The LLMV for succulent shelled beans was 0.02 ppm for each analyte. The LLMV for 

cantaloupe was 0.015 ppm for acequinocyl and 0.01 ppm for acequinocyl-OH. For cherries, 

cucumbers, and caneberries, the LLMV was 0.01 for each analyte.

Conclusions: An adequate HPLC/MS/MS method (Morse Method #Meth-133, revision #3) is

available for enforcing the proposed tolerances, and the residue data from the field trials were 

determined using an adequate modification of this. The method LOQ (based on the LLMV) for 

succulent shelled beans was 0.02 ppm for each analyte. The LOQ (based on the LLMV) for 

cantaloupe was 0.015 ppm for acequinocyl and 0.01 ppm for acequinocyl-OH. For cherries, 

cucumbers, and caneberries, the LOQ (based on the LLMV) was 0.01 for each analyte. 

860.1360 Multiresidue Methods

Acceptable MRM method testing data were submitted for acequinocyl and acequinocyl-OH, and 

these data were forwarded to the U.S. FDA for further evaluation (Memo, S. Levy, 18-FEB2004; DP# 298917). Acequinocyl was adequately recovered from fortified apples using Method 

302, E1 + C1 with GC/electron-capture detector (ECD), but was not recovered using Method 303 

or 304 due to poor recoveries from the Florisil cleanup. Acequinocyl-OH was completely 

recovered from fortified apples using Method 402, E1, or E2 + C1 with GC/ECD, but was not 
Acequinocyl Summary of Analytical Chemistry and Residue Data DP#: 389989

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recovered using Methods 302, 303, or 304.

860.1380 Storage Stability

A summary of storage stability data are given below for each newly proposed crop.

Succulent beans

Samples of succulent bean seeds without pods were stored frozen for up to 824 days prior to 

analysis and 802 days for bean plants with pods. The freezer storage stability of acequinocyl and 

acequinocyl-OH was assessed concurrently in this study, with samples spiked at 0.1 ppm. 

Results from the concurrent storage stability study indicate that residues of acequinocyl and 

acequinocyl-OH are stable for up to 781 days in/on bean plants with pods (seed removed) and 

that residues of acequinocyl-OH are stable for up to 757 days in/on succulent bean seeds without 

pods and that acequinocyl residues decline ~50% during this interval in/on succulent bean seeds. 

Residues were adjusted to account for the decline during storage.

Caneberry

Treated caneberry samples were stored frozen for up to 719 days prior to extraction. All samples 

were analyzed within 1 day of extraction. The freezer storage stability of acequinocyl and 

acequinocyl-OH residues in/on caneberries was assessed concurrently in this study, with samples 

spiked at 0.1 ppm. The mean corrected residue recoveries (corrected for concurrent recoveries 

from freshly spiked samples) of acequinocyl and acequinocyl in samples stored frozen for 685 

days were 84% (n=3, SD=5 %) and 80% (n=3, SD=3%), respectively. As such, there are no 

concerns with the stability of acequinocyl and acequinocyl-OH over time in/on caneberry

samples from this study.

Cantaloupe

Treated cantaloupe samples were stored frozen for up to 751 days prior to extraction. 

Cantaloupe fruit storage stability samples were fortified with acequinocyl and acequinocyl-OH, 

each at 0.1 ppm. Storage stability samples were analyzed 712 days after fortification. Storage 

stability cantaloupe fruit samples averaged 66 ± 2% (n=3) for acequinocyl and 77 ± 3% (n=3) for 

acequinocyl-OH. Concurrent storage stability recovery spikes averaged 98 ± 3% for acequinocyl 

and 84 ± 4% for acequinocyl-OH. Results from the concurrent storage stability study indicate 

that residues of acequinocyl and acequinocyl-OH are stable for up to 712 days in/on cantaloupe 

and that acequinocyl residues decline to ~67% during this interval. Residues were adjusted to 

account for the decline during storage.

Cherry

Treated cherry samples were stored frozen for up to 874 days (~29 months). Results from the 

concurrent storage stability study indicate that residues of acequinocyl and acequinocyl-OH are 

stable for up to 874 days in/on cherries. The mean corrected residue recoveries (corrected for 

concurrent recoveries from freshly spiked samples) of acequinocyl-OH in samples stored frozen 

for 874 days were 80% (n=3, SD=7). There are no concerns with the stability of acequinocyl 

over time in/on cucumber samples from this study. 

Cucumbers

Treated cucumber samples were stored frozen for up to 799 days prior to extraction. The freezer 

storage stability of acequinocyl and acequinocyl-OH residues in/on cucumbers was assessed 

concurrently in this study, with samples spiked at 0.1 ppm. The mean corrected residue 
Acequinocyl Summary of Analytical Chemistry and Residue Data DP#: 389989

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recoveries (corrected for concurrent recoveries from freshly spiked samples) of acequinocyl and 

acequinocyl-OH in samples stored frozen for 741 days were 59% (n=3, SD=6 %) and 116% 

(n=3, SD=5%), respectively. There are no concerns with the stability of acequinocyl-OH over 

time in/on cucumber samples from this study. However, residues of acequinocyl in/on 

cucumbers declined significantly over a period of 741 days. As such, residues of acequinocyl 

in/on treated cucumber samples were corrected for storage dissipation.

The storage durations and conditions of samples from the crop field trial studies submitted to 

support this petition are presented in Table 4. 

Table 4. Summary of Storage Conditions and Durations of Samples from Crop Field Trial Studies. 

Matrix 

Storage

Temperature

(°C)

Actual Storage

Duration Interval of Demonstrated Storage Stability

Succulent bean 

seeds without 

pods

<-20

802 days

(26.4 months)

Results from the concurrent storage stability study indicate that 

residues of acequinocyl-OH are stable for up to 757 days and that 

acequinocyl residues decline ~50% during this interval.

Succulent bean 

plants with pods

824 days

(26.4 months)

Results from the concurrent storage stability study indicate that 

residues of acequinocyl and acequinocyl-OH are stable for up to 781 

days.

Caneberries -20 719 days

(23.6 months)

Results from the concurrent storage stability study indicate that 

residues of acequinocyl and acequinocyl-OH were stable for up to 

685 days.

Cantaloupe <-20 751days

(≤26.4 months)

Results from the concurrent storage stability study indicate that 

residues of acequinocyl-OH are stable for up to 712 days and that 

acequinocyl residues decline to ~67% during this interval.

Cherry <-20 874 days

(≤28.7 months)

Results from the concurrent storage stability study conducted on 

cherries indicate that residues are stable for up to 874 days.

Cucumbers -20 799

Corrected recoveries of acequinocyl residues from cucumbers stored 

frozen for up to 741 days ranged from 53–64% (mean ± SD = 59 ± 

6%) indicating dissipation of residues. Results from the concurrent 

storage stability study indicate that residues of acequinocyl-OH were 

stable for up to 741 days.

Conclusions: The submitted concurrent storage stability data for the above-listed crops is 

adequate to support the storage intervals and conditions incurred by the field trial studies. 

860.1480 Meat, Milk, Poultry, and Eggs

Based on the available goat and poultry metabolism data and the previously calculated dietary

exposures of livestock to acequinocyl residues, HED previously set livestock commodities on 

cattle, goat, horse, and sheep fat and liver at 0.02 ppm (for more details, see: S. Levy, 10-MAR2004; D284757; and 05-SEP-2007; D330439). Exposure of poultry and hog to acequinocyl is 

not expected, as there are no established or proposed tolerances on poultry or hog feedstuffs. 

The maximum reasonable dietary burdens (MRDBs) of livestock to acequinocyl residues were 

previously calculated to be 0.72 ppm for beef cattle and 0.47 ppm for dairy cattle. 

As cowpea forage and hay are significant feedstuff for livestock (dairy cattle only), the MRDB

of acequinocyl was recalculated for this petition using the Agency’s most recent guidance on 

constructing reasonably balanced livestock diets (Science Advisory Council for Chemistry

(ChemSAC) memo, 30-JUN-2008). The beef cattle MRDBs did not need to be recalculated as 
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cowpea forage and hay are not beef feed items. The recalculated MRDB for dairy cattle is 1.73

ppm (Table 5). 

Table 5. Calculation of Dietary Burdens of Acequinocyl Residues for Livestock.

Feedstuff Dietary 

Component

% Dry 

Matter1 % Diet1 Residues(ppm)

2

Dietary Contribution 

(ppm)

3

Dairy Cattle

Cowpea, forage R 30 20 2.59 1.73

Apple, wet pomace CC 40 10 0.01 0.0025

TOTAL BURDEN 100 1.73

1

Potential dietary burdens for livestock were determined using recent Agency guidance on calculating 

reasonably balanced diets for livestock (memo, 30-JUN-2008).

2 The tolerance level for wet apple pomace was used and the HAFT was used for cowpea forage.

3 Contribution = ([tolerance (or HAFT)/% DM] X % diet) for dairy cattle.

Dairy cattle feeding study (previously reviewed: 45651610.de2)

In a ruminant feeding study, three groups of lactating dairy cows (4/group) were dosed orally 

twice a day for 28 consecutive days with gelatin capsules containing acequinocyl at target doses 

equivalent to 5, 15, and 50 ppm (5 DG, 15 DG, and 50 DG) in the feed on a dry weight basis. 

Based on the average daily dietary intake, the actual dose levels were equivalent to 4.9, 14.9, and 

48.6 ppm of acequinocyl in the diet. 

The LOQ for combined acequinocyl residues is 0.02 ppm in milk and all tissues. The limits of 

detection (LODs) for both analytes were not reported. However, the LODs for each analyte have 

been estimated to be 0.001 ppm in milk, 0.002 ppm in muscle and fat, and 0.005 ppm in liver and 

kidneys. With the exception of two fat samples, residues of acequinocyl were <LOD in all 

samples of milk and tissues from all three dose groups. Acequinocyl residues above the LOD 

were found in samples of milk and tissues from each dose group, with the exceptions of kidney

and muscle samples from the low dose group, which had residues <LOD. In milk, the combined 

residues of acequinocyl and acequinocyl-OH (expressed in parent equivalents) were <0.002-

0.003 ppm for the 5 ppm DG, <0.001-<0.005 ppm for the 15 ppm DG, and <0.003-0.013 ppm 

for the 50 ppm DG. Residues appeared to plateau by Study Day 4. Combined residues were 

<LOQ in all milk samples. In liver, combined residues were <0.014-<0.032 ppm for the 5 ppm 

DG, <0.022-<0.037 ppm for the 15 ppm DG, and <0.059-<0.089 ppm for the 50 ppm DG. In 

kidneys, combined residues were <0.01 ppm for the 5 ppm DG, <0.010-<0.014 ppm for the 15 

ppm DG, and <0.019-<0.040 ppm for the 50 ppm DG. In muscle, combined residues were 

<0.004 ppm for the 5 ppm DG, <0.004-<0.006 ppm for the 15 ppm DG, and <0.007-<0.008 ppm 

for the 50 ppm DG. In fat, combined residues were <0.006-<0.013 ppm for the 5 ppm DG, 

<0.018-<0.030 ppm for the 15 ppm DG, and <0.044-<0.113 ppm for the 50 ppm DG.

For the 5, 15 and 50 DGs, the average combined residues were respectively <0.002, <0.003, and 

<0.006 ppm in milk; <0.023, <0.030, and <0.070 ppm in liver; <0.010, <0.012, and <0.034 ppm 

in kidneys; <0.004, <0.005, and <0.007 ppm in muscle; and <0.009, <0.022, and <0.075 ppm fat. 

The combined acequinocyl residues increased linearly with increased feeding level in liver and 

fat, but there was no linear relationship between feeding level and residues in the other tissues 

and milk.

Considering only the LOQ (0.01 ppm) for the two analytes, the combined residues were <LOQ 
Acequinocyl Summary of Analytical Chemistry and Residue Data DP#: 389989

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(<0.02 ppm) in milk and muscle samples from all three dose groups, the kidney samples from the 

5 and 15 ppm DG and fat samples from the 5 DG. Residues above the combined LOQ were 

found in liver at all three dose groups, fat samples from the 15 and 50 DG, and in kidney from 

the 50 ppm DG.

Table 6. Summary of Milk and Tissue Residue Data from Ruminant Feeding Study with Acequinocyl.

Matrix Feeding 

Level (ppm) Study Days1 Combined Acequinocyl Residue Levels (ppm)2

n Min. Max. Mean Std. Dev.

Milk 5 4, 8, 12, 16, 20, 24, 28 28 <0.002 <0.003 <0.002 0.0003

15 4, 8, 12, 16, 20, 24, 28 28 <0.002 <0.005 <0.003 0.0009

50 4, 8, 12, 16, 20, 24, 28 28 <0.002 0.013 <0.006 0.0021

Liver 5 28 4 <0.014 <0.032 <0.023 0.007

15 28 4 <0.022 <0.037 <0.030 0.006

50 28 4 <0.059 <0.089 <0.070 0.014

Kidney 5 28 4 <0.010 <0.010 <0.010 0

15 28 4 <0.010 <0.014 <0.012 0.002

50 28 4 <0.019 <0.040 <0.034 0.009

Muscle 5 28 4 <0.004 <0.004 <0.004 0

15 28 4 <0.004 <0.006 <0.005 0.001

50 28 4 <0.007 <0.008 <0.007 0.0005

Fat 5 28 3 <0.006 <0.013 <0.009 0.004

15 28 4 <0.018 0.030 <0.022 0.005

50 28 4 <0.044 <0.113 <0.075 0.033

1 As residues in milk appeared to plateau by Study Day 4, collected samples from Days 4-28 were used to calculate 

average residues. Tissue samples were collected from animal sacrificed within 24 hours of receiving the final dose.

2 The LOQ for combined acequinocyl residues (expressed in parent equivalents) is 0.02 ppm in all matrices; the 

combined LOD was estimated by the reviewer to be 0.004 ppm in fat and muscle, and 0.010 ppm in liver and kidney. 

Values proceeded by a “<” indicate that residues of one or more of the analytes were below the LOD.

Expected secondary residues in meat and milk

To determine the need for tolerances for acequinocyl residues in tissues, the anticipated 

secondary residues in cattle matrices were estimated using transfer coefficient factors calculated 

from the maximum residues of acequinocyl observed in the ruminant feeding study. Only the 

tissue matrices with detectable residues (>0.02 ppm) are shown below in Table 7. The transfer 

coefficients (calculated as residue-level-to-feed ratios) are also show in Table 7. 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 (Table 8). 

Table 7. Residue-Level-to-Feed Ratios (Transfer Coefficients) in Dairy Tissues.

Matrix Maximum Residue 

(ppm)

Feeding Level, ppm Transfer Coefficient1

Liver

<0.032 5 <0.0064

<0.037 15 <0.002 Ave. = <0.003

<0.089 50 <0.0018

Kidney <0.040 50 <0.0008

Fat 0.030 15 0.002 Ave. = <0.002

<0.113 50 <0.0023

1

 Calculated from the maximum residues divided by the dose level.
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Table 8. Expected Secondary Residues in Meat.

Matrix

Dietary 

burden 

(ppm)

Secondary 

Residues 

(ppm)

1

Established 

Tolerance 

(ppm)

HEDRecommended 

Tolerance 

(ppm)

Notes to RD

Liver

1.73

0.0052 0.022-- A new tolerance of 0.02 ppm in/on 

cattle, goat, horse, and sheep meat 

byproducts should be established to 

cover residues in liver and kidney.

Kidney 0.0014 - 0.021

Fat 0.0035 0.02 0.02 The currently-established tolerance is 

adequate.

1

 Calculated from dietary burden x average transfer coefficient from Table 7. 

2

 The established liver tolerance should be removed in 40 CFR §180.599 with the establishment of a new meat

byproducts tolerance.

Conclusions: The feeding study data indicate that the currently established tolerance level at 

0.02 ppm for residues in cattle, goat, horse, and sheep fat are appropriate. The established 0.02-

ppm residue level in cattle, goat, horse, and sheep liver are appropriate; however, the commodity

definition should be changed to “meat byproducts” rather than “liver.” With the establishment of 

the cattle, goat, horse, and sheep tolerance in meat byproducts, RD should remove the tolerance 

for liver. Furthermore, the meat byproducts tolerance of 0.02 ppm is adequate to cover residues 

in the kidney of cattle, goats, horses, and sheep. A revised Section F should be submitted.

860.1500 Crop Field Trials

DER References: 48462901.der (bean, succulent shelled)

48462902.der (caneberry)

48462903.der (cantaloupe) 

48462904.der (cherry)

48462905.der (cucumber)

No new data were submitted to support tolerances on succulent soybean vegetables, low-growing 

berry 13-07G crop subgroup, or small fruit vine climbing subgroup 13-07F, except fuzzy

kiwifruit. A summary of the data submitted for the proposed new crops can be found below.

Succulent soybean vegetable

No new data were submitted for this crop; however, an edible-podded bean tolerance is 

established in 40 CFR §180.599 at 0.25 ppm. IR-4 has requested that this tolerance be extended 

to support a succulent soybean vegetable tolerance.

Conclusion: HED recommends that a tolerance at 0.25 ppm in/on edible-podded beans should 

be extended to soybean, vegetable, succulent.

Low-growing berry subgroup 13-07G

No new data were submitted for this crop subgroup; however, a strawberry tolerance is 

established in 40 CFR §180.599 at 0.40 ppm. IR-4 has requested that this tolerance be extended 

to support a low-growing berry 13-07G subgroup crop tolerance.

Conclusions: HED recommends that the established strawberry tolerance be extended to the 

low-growing berry 13-07G crop subgroup. The OECD Calculator shows that the data support a 

tolerance of 0.40 ppm for the low-growing berry subgroup 13-07G (which includes 

strawberries). Canada has a MRL of 0.5 ppm in/on strawberries. In order to harmonize with 
Acequinocyl Summary of Analytical Chemistry and Residue Data DP#: 389989

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Canada, HED recommends establishing a tolerance of 0.50 ppm for this subgroup. A revised 

Section F should be submitted. With establishment of this crop subgroup, the strawberry

tolerance in 40 CFR §180.599 should be removed.

Small fruit vine climbing subgroup 13-07F, except fuzzy kiwifruit

No new data were submitted for this crop subgroup; however, a grape tolerance is established in 

40 CFR §180.599 at 1.6 ppm. IR-4 has requested that this tolerance be extended to support small 

fruit vine climbing subgroup 13-07F, except fuzzy kiwifruit tolerance.

Conclusions: HED recommends that the established grape tolerance be extended to small fruit 

vine climbing subgroup 13-07F, except fuzzy kiwifruit at 1.6 ppm. With establishment of this 

crop subgroup, the grape tolerance in 40 CFR §180.599 should be removed.

IR-4 submitted field trial data in support of the proposed uses on succulent shelled beans,

caneberry, cantaloupe, cherry, and cucumber. The results of the field trials are summarized in 

Table 9. 

Table 9. Summary of Residue Data from Crop Field Trials with Acequinocyl.

Commodity

Total Applic. 

Rate

(lb ai/A)

PHI 

(days)

Total Acequinocyl and Acequinocyl-OH Residues (ppm)

n Min. Max. LAFT1 HAFT1 Median Mean Std. 

Dev.

BEAN, SUCCULENT SHELLED (proposed use = 0.6 lb ai/A total application rate, 7-day PHI)2

Bean seeds 

without pods

0.610-0.911 6-8 14 <0.06 <0.125 <0.06 <0.173 0.06 0.081 0.04

Bean plants with 

pods

0.610-0.911 6-9 14 <0.34 3.03 <0.345 2.59 1.69 1.58 0.96

CANEBERRY, SUBGROUP 13-07A (proposed use = 0.6 lb ai/A total application rate, 1-day PHI)3

Raspberry 0.584-0.606 1 5 <0.13 2.28 <0.28 1.91 0.801 0.958 0.711

Blackberry 0.607-0.612 1 2 0.564 0.785 0.606 0.675 0.606 0.640 --

MELON SUBGROUP 9A (proposed use = 0.6 lb ai/A total application rate, 1-day PHI)4

Cantaloupe 0.602-0.833 1 16 <0.025 <0.122 <0.027 <0.089 <0.039 0.040 0.01

CHERRY (proposed use = 0.6 lb ai/A total application rate, 7-day PHI)5

Cherry, tart 0.6042-0.6211 6-7 12 <0.160 <0.481 <0.170 <0.461 0.290 0.319 0.115

Cherry, sweet 0.5836-0.6204 6-7 12 <0.060 <0.216 <0.062 <0.216 0.135 0.140 0.054

CUCUMBER (proposed use = 0.6 lb ai/A total application rate, 1-day PHI)6

Cucumber, field 0.567-0.625 1 8 <0.02 <0.069 <0.02 <0.061 0.044 0.042 0.018

Cucumber, 

greenhouse

0.597-0.604 1 2 <0.029 <0.093 <0.030 <0.069 0.037 0.049 -

1

 LAFT = lowest-average-field-trial; HAFT = highest-average-field-trial.

2

 Total residues = Acequinocyl (corrected for storage decline where applicable) + Acequinocyl-OH. LOQ = 0.02 ppm for each 

analyte.

3

 Total residues = Acequinocyl + Acequinocyl-OH (corrected for concurrent recovery where applicable). LOQ = 0.01 ppm for 

each analyte.

4

 Total residues = Acequinocyl (corrected for storage decline where applicable) + Acequinocyl-OH. LOQ = 0.015 ppm for 

acequinocyl; 0.01 for acequinocyl-OH.

5

 Total residues = Acequinocyl + Acequinocyl-OH. LOQ = 0.01 ppm for each analyte.

6

 Total residues = Acequinocyl (corrected for storage dissipation) + Acequinocyl-OH. LOQ = 0.01 ppm for each analyte.
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Bean, Succulent Shelled

IR-4 has submitted field trial data for acequinocyl on succulent shelled beans and bean plant with 

the pod (seed removed). Seven bean field trials were conducted in North American Free Trade 

Agreement (NAFTA) Growing Zone 10 (CA; 2 trials), Zone 2 (GA, 2 trials), Zone 5 (OH; 1 

trial), Zone 2 (SC; 1 trial), and Zone 11 (WA; 1 trial) during the 2006 growing season.

At each site, a 1.25 lb/gal SC formulation of acequinocyl was applied to beans as two foliardirected applications at rates of 0.302-0.378 lb ai/A/application, with a 14- to 15- day RTI, for a 

total rate of 0.610-0.680 lb ai/A (except in the case of one CA trial where a third application was 

made for a total rate of 0.911 lb ai/A). Applications were made using ground equipment in spray

volumes of 36-72 gal/A, without a spray adjuvant. Applications were timed so that 

commercially mature succulent bean seed without pods could be collected at a 6- to 8-day PHI 

and commercially mature bean plants with pods (seed removed) could be collected at a 6- to 9-

day PHI. A residue-decline study was not conducted.

Total combined residues of acequinocyl (corrected for decline during storage) and acequinocylOH in/on bean seeds without pods ranged from <0.06-<0.125 ppm, harvested 6-8 days following 

foliar applications of the SC formulation for a total rate of 0.610-0.911 lb ai/A. Total combined 

residues of acequinocyl and acequinocyl-OH in/on bean plants with pods ranged from <0.34-

3.03 ppm, harvested 6-9 days following foliar applications of the SC formulation for a total rate 

of 0.610-0.911 lb ai/A (see Table 9). 

Conclusions: The submitted succulent bean field trial data are acceptable and reflect the use of 

the acequinocyl 1.25 lb/gal SC formulation as two foliar applications for a total rate of 0.610-

0.911 lb ai/A (trial 06-CA*28 reflected three applications of approximately 0.303 lb ai/A, for a 

total of 0.909 lb ai/A), with a 6- to 8-day PHI. 

Total combined residues of acequinocyl (corrected for decline during storage) and acequinocylOH in/on bean seeds without pods ranged from <0.06-<0.125 ppm, harvested 6-8 days following 

foliar applications of the SC formulation for a total rate of 0.610-0.911 lb ai/A. Total combined 

residues of acequinocyl and acequinocyl-OH in/on bean plants with pods ranged from <0.34-

3.03 ppm, harvested 6-9 days following foliar applications of the SC formulation for a total rate 

of 0.610-0.911 lb ai/A. 

The residue data for bean seeds without pods and bean plants with pods were entered separately

into the OECD MRL Calculator. Based on the results of these trials, the appropriate tolerance 

for residues of acequinocyl and acequinocyl-OH in/on bean, succulent shelled is 0.30 ppm and 

cowpea, forage is 6.0 ppm. Typically, forage is harvested before the plant has bloomed. 

However, the label does not specify at what plant stage the product can be applied. The plants 

were harvested and analyzed after the plants were blooming/fruiting. Therefore, HED deems it 

necessary to establish a tolerance on cowpea, hay as well. There is typically a 3-fold drying 

factor between forage and hay. As HED is recommending for a tolerance for residues in/on 

cowpea, forage at 6.0 ppm, a tolerance for residues of acequinocyl and acequinocyl-OH in/on 

cowpea, hay at 18 ppm should be established. A revised Section F should be submitted.

Caneberries

The IR-4 has submitted field trial data for acequinocyl in/on caneberries. Five supervised crop 
Acequinocyl Summary of Analytical Chemistry and Residue Data DP#: 389989

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field trials for acequinocyl in/on raspberries and two supervised crop field trials for acequinocyl 

in/on blackberries were conducted in the U.S. and Canada during the 2007 growing season 

encompassing NAFTA Growing Zones 2 (1 raspberry trial in NJ), 5A (1 raspberry trial in MI), 

10 (1 blackberry trial in CA), and 12 (1 raspberry trial in BC, 1 raspberry trial in OR, and 1 

blackberry trial in OR). At each trial site, acequinocyl (formulated as KanemiteTM 15 SC) was 

applied to caneberries as 2 foliar directed or broadcast applications at rates of 0.289-0.313 

pounds ai/A, with RTIs of 15-23 days, for a total seasonal application rate of 0.584-0.612 pounds 

ai/A. Applications were made in spray volumes ranging from 51-111 gallons/A. No adjuvants 

were used in any of the spray mixtures. Commercially mature berries were harvested at a PHI of 

1 day. At the QC03 trial site, mature berries were harvested at additional PHIs of 0, 4, 6, and 11 

days to assess residue-decline behavior.

Total residues of acequinocyl and acequinocyl-OH (corrected for concurrent recoveries) in/on 

raspberries treated at total rates of 0.584-0.606 pounds ai/A/season and harvested at a PHI of 1 

day ranged from <0.13-2.28 ppm. Total residues of acequinocyl and acequinocyl-OH (corrected 

for concurrent recoveries) in/on blackberries treated at total rates of 0.607-0.612 pounds 

ai/A/season and harvested at a PHI of 1 day ranged from 0.564-0.785 ppm (Table 9). Residuedecline data indicated that total residues of acequinocyl and acequinocyl-OH in/on raspberries 

declined with increasing PHIs.

Conclusions: The supervised crop field trials for acequinocyl in/on caneberries are considered 

scientifically valid. KanemiteTM 15 SC was applied to raspberries and blackberries as 2 foliar 

applications at rates total rates of 0.584-0.612 pounds ai/A/season and harvested commercially

mature caneberries at a PHI of 1 day. Total residues of acequinocyl and acequinocyl-OH 

(corrected for concurrent recoveries) in/on raspberries ranged from <0.13-2.28 ppm. Total 

residues of acequinocyl and acequinocyl-OH (corrected for concurrent recoveries) in/on

blackberries ranged from 0.564-0.785 ppm. Residue-decline data in/on raspberries indicated that 

total residues of acequinocyl and acequinocyl-OH in/on raspberries declined with increasing 

PHIs.

The residue data for raspberries were entered into the OECD MRL Calculator (although field 

trial data were submitted for blackberries, there were not enough data to input into the OECD 

calculator). Note that for caneberries, crop subgroup 13-07A, the representative crop is either 

raspberry or blackberry. A minimum of five trials is required on any one blackberry or any one 

raspberry if a tolerance is sought on “caneberries.” Based on the results of these trials, the 

appropriate tolerance for residues of acequinocyl and acequinocyl-OH in/on “caneberry

subgroup 13-07A” is 4.0 ppm. A revised Section F is requested.

Cantaloupe

IR-4 has submitted field trial data for acequinocyl on cantaloupe. Six cantaloupe trials were 

conducted in NAFTA Growing Zone 2 (SC; 1 trial), Zone 5 (OH, 1 trial), Zone 6 (TX; 1 trial), 

and Zone 10 (NM, AZ, and CA; 3 trials) during the 2007 growing season.

At the trial sites, a 1.25 lb/gal SC formulation of acequinocyl was applied to cantaloupe as two 

broadcast foliar application at rates of 0.299-0.307 lb ai/A/application for a total rate of 0.600-

0.609 lb ai/A (except in the case of one OH trial where a third application was made for a total 

rate of 0.833 lb ai/A). Applications were made at 20- to 21-day RTIs except for the OH trial, 

where the second application was made at a 15-day RTI. Applications were made using ground 
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equipment in spray volumes of 33-49 gal/A, without a spray adjuvant. Applications were timed 

so that the cantaloupe could be collected at a 1-day PHI. A residue-decline study was conducted 

at the NM trial where sampling was conducted at a 0-, 1-, 3-, 6-, and 9- day PHIs.

Total combined residues of acequinocyl (corrected for decline during storage) and acequinocylOH (calculated in parent equivalents) in/on cantaloupe ranged from <0.025-<0.122 ppm, 

harvested 1 day following foliar applications of the SC formulation for a total rate of 0.602-0.833 

lb ai/A (Table 9). The residue-decline trial (PHI = 0, 1, 3, 6, and 9 day) showed that residues 

declined from 0-3 days, then remained <LLMV.

Conclusions: The submitted cantaloupe field trial data are acceptable and reflect the use of the 

acequinocyl 1.25 lb/gal SC formulation as two broadcast foliar applications for a total rate of 

0.600-0.609 lb ai/A (trial -OH*01 reflected three applications for a total of 0.833 lb ai/A), with a 

1-day PHI. .

Total combined residues of acequinocyl (corrected for decline during storage) and acequinocylOH in/on cantaloupe ranged from <0.025-<0.122 ppm, harvested 1 day following foliar 

applications of the SC formulation for a total rate of 0.602-0.833 lb ai/A. The residue-decline 

trial (PHI = 0, 1, 3, 6, and 9 day) showed that residues declined from 0-3 days, then remained 

<LLMV.

The residue data for cantaloupe were entered into the OECD MRL Calculator. Based on the 

results of these trials, the appropriate tolerance for residues of acequinocyl and acequinocyl-OH 

in/on cantaloupe is 0.15 ppm. As cantaloupe is the representative commodity for melon 

subgroup 9A, the tolerance can be expanded to this subgroup. A revised Section F is 

requested.

Cherry

IR-4 has submitted data from 12 cherry field trials on acequinocyl during the 2006 growing 

season. Six tart cherry field trials were conducted in NAFTA Growing Zone 1 (NY; 1 trial), 

Zone 5 (MI, 4 trials), and Zone 9 (CO; 1 trial). Six sweet cherry field trials were conducted in 

NAFTA Growing Zone 5 (MI; 2 trials), Zone 10 (CA, 2 trials), and Zone 11 (WA; 2 trials).

At the trial sites, a 1.25 lb ai/gal SC formulation of acequinocyl was applied as two foliar 

directed applications at a rate of ~0.303 lb ai/A each, for a total of 0.5836-0.6211 lb ai/A. 

The applications were made at 13- to 15-day RTIs and timed so that marketable pitted 

cherries could be collected at an approximately 7-day PHI after the second application. 

Additional samples for decline determination were collected from the MI08 (tart) and CA29 

(sweet) trials at 2- or 3-, 10-, and 14-day PHIs. Applications were made using ground 

equipment in spray volumes of ~40-315 gal/A, without a spray adjuvant.

Total combined residues of acequinocyl and acequinocyl-OH (and per-trial averages) in/on tart 

cherries ranged from <0.160-<0.481 ppm (<0.170-<0.461 ppm), harvested 6-7 days following 

foliar directed applications of the SC formulation for a total rate of 0.6042-0.6211 lb ai/A. Total 

combined residues of acequinocyl and acequinocyl-OH (and per-trial averages) in/on sweet 

cherries ranged from <0.060-<0.216 ppm (<0.062-<0.216 ppm), harvested 6-7 days following 

foliar applications of the SC formulation for a total rate of 0.5836-0.6204 lb ai/A (Table 9). In 
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general, residues were higher in tart cherries than in sweet cherries. Both the tart and sweet 

cherry residue-decline trials (PHI = 0, 2 or 3, 6 or 7, 10, and 14 day) showed that residues 

increased slightly at the first interval, and then declined.

Conclusions: The submitted cherry field trial data (6 trials on tart cherries, 6 trials on sweet 

cherries) are acceptable and reflect the use of the acequinocyl 1.25 lb ai/gal SC formulation as 

two foliar directed applications for a total rate of 0.5836-0.6211 lb ai/A, with a 6-7-day PHI. 

Additional samples for decline determination were collected from two trials at 2 or 3, 6 or 7, 10, 

and 14 days. 

Total combined residues of acequinocyl and acequinocyl-OH (and per-trial averages) in/on tart 

cherries ranged from <0.160-<0.481 ppm (<0.170-<0.461 ppm), harvested 6-7 days following 

foliar directed applications of the SC formulation for a total rate of 0.6042-0.6211 lb ai/A. Total 

combined residues of acequinocyl and acequinocyl-OH (and per-trial averages) in/on sweet 

cherries ranged from <0.060-<0.216 ppm (<0.062-<0.216 ppm), harvested 6-7 days following 

foliar applications of the SC formulation for a total rate of 0.5836-0.6204 lb ai/A. In general, 

residues were higher in tart cherries than in sweet cherries. Both the tart and sweet cherry

residue-decline trials (PHI = 0, 2 or 3, 6 or 7, 10, and 14 day) showed that residues increased 

slightly at the first interval, and then declined.

The residue data for tart and sweet cherries were separately entered into the OECD MRL

Calculator. Based on the results of these trials, the appropriate tolerances for residues of 

acequinocyl and acequinocyl-OH are 1.0 ppm in/on cherry, tart and 0.50 ppm in/on cherry, 

sweet. A revised Section F is requested.

Cucumbers

IR-4 has submitted field trial and greenhouse data for acequinocyl in/on cucumbers. Nine 

supervised crop field trials in/on field cucumbers (pickling and slicing varieties) were conducted 

in the U.S. during the 2007 growing season encompassing NAFTA Growing Zones 2 (2 trials in 

GA, 1 trial in NC), 5 (2 trials in OH), 6 (1 trial in TX) and 10 (2 trials in CA). At each trial site, 

acequinocyl [formulated as KanemiteTM 15 SC] was applied to field cucumbers as 2 foliar 

broadcast or foliar directed applications at rates of 0.263-0.325 pounds ai/A, at RTIs of 19-23 

days, for a total rate of 0.567-0.636 pounds ai/A/season. The applications were made in spray

volumes ranging from 32-77 gallons/A. No adjuvants were used in any of the spray mixtures. 

Commercially mature field cucumbers were harvested at a PHI of 1 day. At the GA*15 trial site, 

field cucumbers were harvested at additional PHIs of 0, 4, 7, and 9 days to assess residue-decline 

behavior.

In addition, two greenhouse cucumber trials were conducted in the U.S. and Canada during the 

2007 growing season encompassing NAFTA Growing Zones 2 (1 trial in NJ) and 5 (1 trial in 

ON). At each trial site, acequinocyl (formulated as KanemiteTM 15 SC) was applied to 

greenhouse cucumbers as two foliar-directed applications at rates of 0.296-0.303 pounds ai/A, at 

RTIs of 19-20 days, for a total rate of 0.597-0.604 pounds/A/season. The applications were 

made in spray volumes ranging from 53-188 gallons/A. No adjuvants were used in any of the 

spray mixtures. Commercially mature greenhouse cucumbers were harvested at a PHI of 1 day. 

At the ON01 trial site, greenhouse cucumbers were harvested at additional PHIs of 0, 3, 7, and 9 

days to assess residue-decline behavior.
Acequinocyl Summary of Analytical Chemistry and Residue Data DP#: 389989

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Total residues of acequinocyl (corrected for storage dissipation) and acequinocyl-OH in/on field 

cucumbers treated at total rates of 0.567-0.625 pounds ai/A/season (636-701 g ai/ha/season) and 

harvested at a PHI of 1 day ranged from <0.02-<0.069 ppm (Table 9). Residue-decline data 

indicated that total residues of acequinocyl and acequinocyl-OH in/on field cucumbers declined 

with increasing PHIs.

Total residues of acequinocyl (corrected for storage dissipation) and acequinocyl-OH in/on 

greenhouse cucumbers treated at total rates of 0.597-0.604 pounds ai/A/season (669-677 g 

ai/ha/season) and harvested at a PHI of 1 day ranged from <0.029-<0.093 ppm (Table 9). 

Residue-decline data indicated that total residues of acequinocyl and acequinocyl-OH in/on 

greenhouse cucumbers declined with increasing PHIs.

Conclusions: The submitted crop field trials for acequinocyl in/on field cucumbers and 

greenhouse cucumbers are considered scientifically valid. KanemiteTM 15 SC was applied to 

field cucumbers as two foliar (broadcast or directed) applications at rates total rates of 0.567-

0.625 lbs ai/A and mature field cucumbers were harvested at a PHI of 1 day. Total residues of 

acequinocyl (corrected for storage dissipation) and acequinocyl-OH in/on field cucumbers 

ranged from <0.02-<0.069 ppm. Residue decline data indicated that total residues of 

acequinocyl and acequinocyl-OH in/on field cucumbers declined with increasing PHIs. 

KanemiteTM 15 SC was also applied to greenhouse cucumbers as two foliar (broadcast or 

directed) applications at total rates of 0.597-0.604 lbs ai/A and mature greenhouse cucumbers 

were harvested at a PHI of 1 day. Total residues of acequinocyl (corrected for storage 

dissipation) and acequinocyl-OH in/on greenhouse cucumbers ranged from <0.029-<0.093 ppm. 

Residue decline data indicated that total residues of acequinocyl and acequinocyl-OH in/on 

greenhouse cucumbers declined with increasing PHIs.

The residue data for field and greenhouse cucumbers were entered into the OECD MRL

Calculator (see ChemSAC minutes, 19-OCT-2011). Running the OECD MRL Calculator both 

with and without the greenhouse cucumber data resulted in the same tolerance level of 0.15 ppm.

Based on the results of these trials, the appropriate tolerance for residues of acequinocyl and 

acequinocyl-OH is 0.15 ppm in/on cucumber.

860.1520 Processed Food and Feed

There are no processed food/feed items associated with the proposed uses. Therefore, data 

requirements for this guideline are not relevant to this tolerance petition.

860.1650 Submittal of Analytical Reference Standards

Analytical reference standards for acequinocyl and acequinocyl-OH are currently available at the 

EPA National Pesticide Standards Repository (electronic communication with Theresa Cole, 31-

OCT-2011) with expiration dates of June, 2012. 

860.1850/1900 Confined and Field Accumulation in Rotational Crops

The proposed uses under this petition include succulent soybeans, berries (subgroup 13-07G), 

succulent shelled beans, cowpea forage, cucumbers, and melons (subgroup 9A) which are 

typically rotated crops. An acceptable confined rotational crop study was previously submitted 

(Memo, S. Levy, 25-JUN-2008; DP#s 351336 & 353313) in support of uses on strawberries. 
Acequinocyl Summary of Analytical Chemistry and Residue Data DP#: 389989

Page 20 of 30

The study results (47332501.der) showed the extent and nature of the residue uptake by crops 

(lettuce, turnip and wheat) planted 30-, 120- and 365-days post-application in soil treated with 

14C-acequinocyl at 0.60 lb ai/A (1x maximum registered/proposed seasonal application rate to 

rotated crops). The available data support a 30-day PBI for all non-labeled crops, which is 

reflected on the proposed label.

860.1550 Proposed Tolerances

Tolerances are currently established under 40 CFR §180.599(a) for the combined residues of 

acequinocyl and its metabolite, 2-dodecyl-3-hydroxy-1,4-naphthoquinone, expressed as 

acequinocyl equivalents, in/on a number of plant and livestock commodities. Tolerances for 

plant commodities range from 0.02 ppm (tree nuts and pistachios) to 30 ppm (citrus oil), and 

tolerances for livestock commodities are established at 0.02 ppm in the fat and liver of cattle, 

goat, horse, and sheep. Compliance with the tolerance levels specified below in Table 10 is to be 

determined by measuring acequinocyl and its metabolite, 2-dodecyl-3-hydroxy-1,4-

naphthoquinone, expressed as acequinocyl equivalents.

There are currently no established Codex, Canadian, or Mexican MRLs for acequinocyl residues 

in/on cucumbers or caneberries. Data for these crops were jointly reviewed by the U.S. and 

Canada. The data support tolerance levels of 0.15 ppm and 0.40 ppm, respectively. These levels 

are harmonized between the U.S. and Canada.

 

Canada has a MRL of 0.5 ppm for residues in/on strawberries. The OECD Calculator shows that 

the data support a tolerance of 0.40 ppm for residues in/on the low-growing berry subgroup 13-

07G (which includes strawberries); however, in order to harmonize with Canada, HED 

recommends establishing a tolerance of 0.50 ppm for residues in this subgroup. Canada also has 

a MRL for residues of 0.02 ppm in/on meat byproducts of cattle, goat, horse, and sheep. HED is 

recommending for the same tolerance level as Canada; therefore, harmonization will not be an 

issue.

Table 10. Tolerance Summary for Acequinocyl.

Commodity Proposed Tolerance 

(ppm)

HEDRecommended 

Tolerance (ppm)

Comments; 

Correct Commodity Definition

Soybean, vegetable, succulent 0.25 0.25 Established edible-podded 

bean tolerance extended to 

soybean, vegetable, succulent.

Low-growing berry subgroup 

13-07G

0.4 0.50 Established strawberry

tolerance extended for a 

subgroup tolerance. With 

establishment of this subgroup 

tolerance, the strawberry 

tolerance should be removed.

Small fruit vine climbing subgroup 13-

07F, except fuzzy kiwifruit

1.6 1.6 Established grape tolerance 

extended for a subgroup 

tolerance. With establishment 

of this subgroup tolerance, the 

grape tolerance should be 

removed.

Bean, succulent shelled 0.15 0.30
Acequinocyl Summary of Analytical Chemistry and Residue Data DP#: 389989

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Table 10. Tolerance Summary for Acequinocyl.

Commodity Proposed Tolerance 

(ppm)

HEDRecommended 

Tolerance (ppm)

Comments; 

Correct Commodity Definition

Cowpea, forage 9.0 6.0

Cowpea, hay -- 18

Caneberry subgroup 13-07A 4.5 4.0

Melon subgroup 9A 0.06 0.15

Cucumber 0.15 0.15

Cherry

0.8 1.0 Cherry, tart

-- 0.50 Cherry, sweet

Liver of cattle, goat, horse, and sheep1-- 0.02 Meat byproducts of cattle, 

goat, horse and sheep

1

 A tolerance of 0.02 ppm is already established under 40 CFR §180.599; however, the commodity definition should be changed

to meat byproducts to cover residues in liver and kidney.

Conclusions: The petitioner should submit a revised Section F with the appropriate commodity 

definitions and/or HED-recommended tolerance levels listed in Table 15. Furthermore, the 

Section F should state the following (as it appears in 40 CFR §180.599): “Tolerances are 

established for residues of acequinocyl, including its metabolites and degradates, in or on the 

commodities in the table below. Compliance with the tolerance levels specified below is to be 

determined by measuring only the sum of acequinocyl [2-(acetyloxy)-3-dodecyl-1,4-

naphthalenedione] and its metabolite, 2-dodecyl-3-hydroxy-1,4-naphthoquinone, calculated as 

the stoichiometric equivalent of acequinocyl, in or on the commodity.” A revised Section F 

should be submitted.

 

References

DP#: 297872

Subject: Acequinocyl. Report of the Metabolism Assessment Review Committee 

(MARC). Meeting Date: 17-DEC-2003.

From: S. Levy/P. Terse

Dated: 07-JAN-2004

MRID: None

DP#: 298917

From: S. Levy

Dated: 18-FEB-2004

MRID: 45651603

DP#s: 284757, 290204, 286425

Subject: Acequinocyl. Registration for Use on Pome Fruits, Citrus, Almonds, Pistachios, 

and Strawberry. Summary of Analytical Chemistry and Residue Data.

From: S. Levy

Dated: 10-MAR-2004

MRID(s): 46602001-46602003

DP#: 321753
Acequinocyl Summary of Analytical Chemistry and Residue Data DP#: 389989

Page 22 of 30

Subject: Acequinocyl. Response to Submission of MRID#s 46602001, 46602002 and 

46602003 by Morse Laboratories Addressing a Need for Confirmation of 

Acequinocyl in Fruits, Almonds and Livestock Tissues.

From: D. Soderberg and S. Levy

Dated: 23-MAY-2006

MRID(s): 46602001-46602003

DP#s: 330439, 337218, 337472

Subject: Acequinocyl. Petitions for Uses on Tree Nuts and Grapes. Summary of

Analytical Chemistry and Residue Data.

From: S. Levy

Dated: 05-SEP-2007

MRID(s): 46776602, 47032402, & 46952301

DP#s: 351336 & 353313

Subject: Acequinocyl; Review of Petitioner’s Amendment Dated 28-JUN-2008 Submitted 

in Response to the Health Effects Division (HED) Memoranda, DP# 284757 

(dated 10-MAR-2004).

From: S. Levy

Dated: 25-JUN-2008

MRID: 47332501

DP#: 380302

Subject: Acequinocyl; Response to the Health Effects Division (HED) Review of 25-JUN2008 (Memoranda, DP#s D351336 & D353313).

From: S. Levy

Dated: 25-AUG-2010

MRID(s): 48016603-48016605

Attachments: 

International Residue Limit Status (IRLS) Sheet.

Appendix I -Tolerance Assessment Calculations.

RDI: G. Kramer (02-NOV-2011); RAB1 Chemists (09-NOV-2011)

S. Levy:S-10953:PY1:(703)305-0783:7509P
Acequinocyl Summary of Analytical Chemistry and Residue Data DP#: 389989

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IRLS Sheet.

Acequinocyl (PC Code 006329; 10/28/2011)

Summary of U.S. and International Tolerances and Maximum Residue Limits 

Residue Definition:

U.S. Canada Mexico2 Codex3

40 CFR 180.599

Plants/Livestock: sum of acequinocyl [2-

(acetyloxy)-3-dodecyl-1,4-

naphthalenedione] and its metabolite, 2-

dodecyl-3-hydroxy-1,4-naphthoquinone, 

calculated as the stoichiometric equivalent 

of acequinocyl

2-(acetyloxy)-3-dodecyl1,4-naphthalenedione, 

including the metabolite 

2-dodecyl-3-hydroxy-1,4-

naphthalenedione

None

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

U.S. Canada Mexico2 Codex3

Soybean, vegetable, succulent 0.25

Low-growing berry subgroup 

13-07G 0.40 0.5 strawberries

Small fruit vine climbing subgroup 

13-07F, except fuzzy kiwifruit 1.6

Bean, succulent shelled 0.30

Cowpea, forage 6.0

Cowpea, hay 18

Caneberry subgroup 13-07A 4.0

Melon subgroup 9A 0.15

Cucumber 0.15

Cherry, sweet 0.50

Cherry, tart 1.0

Meat byproducts of cattle, goat, 

horse, and sheep 0.02

0.02 Meat byproducts of 

cattle, goat, horse, and 

sheep

Completed: M. Negussie; 10/31/2011

1

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

not those proposed by the applicant.

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

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

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

fat portion of the sample. MRLs indicated as proposed have not been finalized by the CCPR and the CAC.
Acequinocyl Summary of Analytical Chemistry and Residue Data DP#: 389989

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Appendix I. Tolerance Assessment Calculations.

Succulent Shelled Beans

The submitted U.S. residue data for succulent shelled beans (seeds without pods) and succulent 

bean plants with pods (7 data points each) were entered into the OECD MRL Calculator in order 

to determine appropriate tolerance levels.

Compound

Crop

Region / Country

GAP

Total number of data (n)

Percentage of censored data

Number of non-censored data

Lowest residue

Highest residue

Median residue

Mean

Standard deviation (SD)

Correction factor for censoring 

(CF)

Proposed MRL estimate

- Highest residue

- Mean + 4 SD

- CF x 3 Mean

Unrounded MRL

Rounded MRL

Acequinocyl

Bean, succulent 

shelled

(seeds w/out pods )

USA

0.610-0.911

7

0%

7

0.060

0.173

0.060

0.081

0.043

1.000

0.173

0.251

0.243

0.251

0.3

Residues (mg/kg)

0.060

0.060

0.173

0.095

0.060

0.060

0.060
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Compound

Crop

Region / Country

GAP

Total number of data (n)

Percentage of censored data

Number of non-censored data

Lowest residue

Highest residue

Median residue

Mean

Standard deviation (SD)

Correction factor for censoring 

(CF)

Proposed MRL estimate

- Highest residue

- Mean + 4 SD

- CF x 3 Mean

Unrounded MRL

Rounded MRL

Residues 

(mg/kg)

0.527

1.690

2.590

2.460

0.952

0.345

2.510

Acequinocyl

Cowpea forage

(bean plants 

w/pods)

USA

0.610-0.911

7

0%

7

0.345

2.590

1.690

1.582

0.975

1.000

2.590

5.481

4.746

5.481

6
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Caneberry Subgroup 13-07A

The submitted U.S. residue data for raspberry (5 data points) and blackberry (2 data points) were 

entered into the OECD MRL Calculator in order to determine an appropriate crop group 

tolerance level.

Compound

Crop

Region / Country

GAP

Total number of data (n)

Percentage of censored data

Number of non-censored data

Lowest residue

Highest residue

Median residue

Mean

Standard deviation (SD)

Correction factor for censoring 

(CF)

Proposed MRL estimate

- Highest residue

- Mean + 4 SD

- CF x 3 Mean

Unrounded MRL

Residues (mg/kg)

0.280

1.910

1.474

0.325

0.801

Acequinocyl

Raspberries

USA

0.584-0.612

5

0%

5

0.280

1.910

0.801

0.958

0.717

1.000

1.910

3.827

2.874

3.827

4
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Melon Subgroup 9A

The submitted U.S. residue data for cantaloupe (8 data points) were entered into the OECD MRL

Calculator in order to determine an appropriate crop group tolerance level.

Compound

Crop

Region / Country

GAP

Total number of data (n)

Percentage of censored data

Number of non-censored data

Lowest residue

Highest residue

Median residue

Mean

Standard deviation (SD)

Correction factor for censoring 

(CF)

Proposed MRL estimate

- Highest residue

- Mean + 4 SD

- CF x 3 Mean

Unrounded MRL

Residues (mg/kg)

0.027

0.047

0.039

0.039

0.061

0.027

0.030

0.035

Acequinocyl

Melon subgroup 9A

(cantaloupe)

USA

0.602-0.833

8

0%

8

0.027

0.061

0.037

0.038

0.012

1.000

0.061

0.084

0.114

0.114

0.15
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Cucumber

The submitted U.S. residue data for field (8 data points) cucumbers were entered into the OECD 

MRL Calculator in order to determine an appropriate tolerance level. 

Compound

Crop

Region / Country

GAP

Total number of data (n)

Percentage of censored data

Number of non-censored data

Lowest residue

Highest residue

Median residue

Mean

Standard deviation (SD)

Correction factor for censoring 

(CF)

Proposed MRL estimate

- Highest residue

- Mean + 4 SD

- CF x 3 Mean

Unrounded MRL

Residues (mg/kg)

0.020

0.031

0.060

0.058

0.020

0.061

0.056

0.031

0.069

0.030

Acequinocyl

Cucumbers 

 (field and greenhouse)

USA

0.567-0.625

10

0%

10

0.020

0.069

0.044

0.044

0.019

1.000

0.069

0.119

0.131

0.131

0.15
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Cherry

The submitted U.S. residue data for sweet (6 data points) and tart (6 data points) cherries were 

entered into the OECD MRL Calculator in order to determine appropriate tolerance levels.

Compound

Crop

Region / Country

GAP

Total number of data (n)

Percentage of censored data

Number of non-censored data

Lowest residue

Highest residue

Median residue

Mean

Standard deviation (SD)

Correction factor for censoring 

(CF)

Proposed MRL estimate

- Highest residue

- Mean + 4 SD

- CF x 3 Mean

Unrounded MRL

Residues (mg/kg)

0.118

0.151

0.192

0.216

0.105

0.062

Acequinocyl

Cherry, sweet

USA

0.5836-0.6204

6

0%

6

0.062

0.216

0.135

0.141

0.057

1.000

0.216

0.370

0.422

0.422

0.5
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Compound

Crop

Region / Country

GAP

Total number of data (n)

Percentage of censored data

Number of non-censored data

Lowest residue

Highest residue

Median residue

Mean

Standard deviation (SD)

Correction factor for censoring 

(CF)

Proposed MRL estimate

- Highest residue

- Mean + 4 SD

- CF x 3 Mean

Unrounded MRL

Residues (mg/kg)

0.315

0.460

0.461

0.170

0.270

0.240

Acequinocyl

Cherry, tart

USA

0.6024-0.6211

6

0%

6

0.170

0.461

0.293

0.319

0.119

1.000

0.461

0.796

0.958

0.958

1