UNITED STATES ENVIRONMENTAL PROTECTION AGENCY 

WASHINGTON, D.C. 20460 

MEMORANDUM 

18-FEB-2016 

O FFICE O F CllEJ\JICAL SAFETY 

A~D POLLITTION PREVENTION 

SUBJECT: Aldicarb. Review of Residue Chemistry Data Submitted in Response to a 

Generic Data Call-Jn (GDCI). 

PC Code: 098301 

Decision No.: 498310 

Petition No.: NA 

Assessment Type: NA 

TXR No.: NA 

MRJD No.: See MRID table below 

DP Barcode: D425 I 80 

Registration No.: 87895-1 

Regul atory Action: GDCI Review 

Case No.: 0140 

CAS No.: 116-06-3 

40 CFR: § 180.269 

FROM: William H. Donovan, Ph.D., Chemist 

Risk Assessment Branch V 

w.~/4.D~ 

Health Effects Division (7509P) 

THROUGH: Danet1e Drew, Chemis , 

TO: 

Mi chael Metzger, Branc h' f 

Risk Assessment Branch V /VII 

Health Effects Division (7509P) 

Susan Bartow, Chemical Review Manager 

Risk Management and Implementation Branch IV 

Pesticide Re-evaluation Division (7508P) 

Office of Pesticide Programs 

Table A. MRID Summa ry Ta ble For Aldicarb. 

MRIO No. Study Type Comments 

48156901 860. 1500 cotton field trials 4815690 I .der.docx 

48156902 860. 1380 storage stability study 48156902.der.docx 

48156903 860. 1340 analytical methods 48 156903.der.docx 

In response to the aldicarb reregistration data call-in of July 2008 (GDCI-09830 1-27347) that 

requested cotton and sorghum field trial studies along with a supporting storage stability study, 

Bayer CropScience (BCS) submitted the studies listed above in Table A. PRO has requested that 

HED review the studies and determine if the submissions adequately address the relevant data gaps. 

Page I of 9 
Aldicarb OCI Residue Chemistry Review OP# 425 180 

HED has prepared Data Evaluation Records (DERs) for the submitted studies as listed in Table 

A above. This memo summarizes the regulatory implications resulting from review of these 

studies. 

Conclusions 

HED concludes that the submitted studies are scientifically reliable and adequately address the 

intended data gaps. As noted in the aldicarb scoping document (0 398520. C. Olinger et al., 

5116120 12), BCS agreed to cancel the use on sorghum, as announced in a Federal Register notice 

dated October 8, 2008 (Volume 73, Number 196, pp. 58958-58962). Therefore, the data on 

sorghum are no longer required. The new cotton field trial data support the following updates to 

aldicarb tolerances in 40 CFR § 180.269: 

RAC Current Recommended Comment 

Tole rance Tolerance (ppm) 

(ppm) 

Co11011. 0. 10 0.20 Increase based on data in MRID 48156901. 

undelinted seed 

Cotton, gin -- 0.40 Value based on data in MRID 4815690 I. 

byproduct 

Cotton. hulls 0.30 Revoke Commodity covered by the raw agricultural commodity tolerance 

(0266396. C. Swartz. 6/2/2000). 

The tolerance recommendations in this memo are not expected to result in significant changes to 

estimated dietary exposures to aldicarb residues. Although cotton raw agricultural commodities 

(RACs) are livestock feedstuffs, residue transfer to livestock commodities is not expected (i.e. , a 

40 CFR § l 80.6(a)(3) situation applies). A human health risk assessment is forthcoming. 

Detailed Considerations 

Analytical Methods (860.1340) 

48 156903.der.docx 

Bayer CropScience submitted a high performance liquid chromatography method with tandem 

mass spectrometry detection (LC/MS/MS), Method 00851 , for the determination of residues of 

aldicarb and its metabolites aldicarb sulfone and aldicarb sulfoxide in potatoes and oranges. The 

method was used for anal ysis of aldicarb and its metabolites aldicarb sulfone and aldicarb 

sulfoxide in the cotton magnitude of the residue crop field trials and freezer storage stability 

studies. 

Briefly, samples were extracted twice with dichloromethane (OCM):acetone (75:25, v:v) and 

filtered. The extracts were combined and diluted with DCM/acetone. Ethylene glycol was 

added, and the mixture was concentrated, reconstituted in acetonitrile and diluted buffer 

(ammonium acetate and acetic acid diluted with water), and filtered. The filtrate was diluted 10 

times using either the diluted buffer or the dilution mixture containing reserpine as injection 

standard for LC/MS/MS analysis. The method monitors a single ion transition for aldicarb (208 

m/z - 116 m/z), aldicarb sulfone (223 rn/z - 76 rn/z), aldicarb sulfoxide (207 rn/z - I 32 m/z), 

and reserpine (609.3 rn/z - 195. l rn/z). The limit of quantitation (LOQ; determined as the 

lowest level of method validation, LLMV) is 0.0 I ppm for each analyte. 

Page 2of9 
Aldicarb DCI Residue Chemistry Review DP# 425180 

The method was adequately validated using samples of potato, orange pulp, and orange peel 

fortifi ed with each analyte at 0.01and0.10 ppm. Recoveries were generally within the 

acceptable range of 70-1 20% for all matrices and analytes. 

Conclusions 

HED concludes that Method 00851 is suitable for data collection purposes. The LC/MS/MS 

Method, 00851, was adequately validated for determining residues of aldicarb and its metabolites 

aldicarb sulfoxide and aldicarb sulfone in potato, orange peel, and orange pulp. The va lidated 

LOQ is 0.0 I ppm. The analytical procedure used in the storage stability and crop field trial 

studies (MRIDs 48156902 and 4815690 I , respecti vely) has been successfully validated for 

aldicarb in tenns of specificity, linearity, precision, accuracy, and LOQ. 

Storage Stability (860.1380) 

48 I 56902.dcr.docx 

Bayer CropScience submitted a storage stability study with aldicarb and its metabolites aldicarb 

sulfoxide and aldicarb sulfone in/on cotton undelinted seed and gin byproducts. Samples of 

untreated commodities were fortified separately with each analyte at 0. 10 ppm, placed in frozen 

storage (:S-20 °C), and analyzed at storage intervals of - 0, 1, 1.3 (seed only), 2, 4, and 5 months 

(0, 27-28, 38 (seed), 55-56, 120- 12 1, and 148-152 days). Because decline was observed in/on 

cotton undelinted seed for residues of all three analytes following I month of storage, additional 

samples of cotton undelinted seed were prepared midway through the study and were analyzed at 

weekly storage intervals of - 0, I, 2, 3, 4, and 7 weeks (8, 15, 22, 28, and 47 days) to more 

accurately monitor loss on storage. 

Conclusions 

The storage stability study with cotton is considered scientifically acceptable. In the 5-month 

study for cotton undelinted seed, residues of aldicarb, aldicarb sulfoxide, and aldicarb sulfone 

declined fo llowing I month of frozen storage, and generally appeared to stabilize at subsequent 

storage intervals. In the 7-week study for undelinted seed, loss on storage was observed for 

residues of all three analytes at storage intervals > 15 days. When the results for both the 5-

month and the 7-week studies are combined, the average recoveries for residues of aldicarb, 

aldicarb sulfoxide, and aldicarb sulfone in/on cotton undelinted seed at all storage intervals> 15 

days were 43-46% (overall average recovery for all three anal ytes of - 44%). The data for cotton 

gin byproducts indicate that residues of aldicarb were stable during frozen storage for up to 4 

months but declined by the 5-month storage interval (40% recovery), while residues of aldicarb 

sulfoxide and aldicarb sulfone were stable for up to 5 months. 

The submitted storage stability data indicate that correction for loss on storage is needed for 

residues of aldicarb, aldicarb sul foxide, and aldicarb sulfone in/on cotton undelinted seed stored 

frozen for > 15 days (44% recovery] and for residues of aldicarb in/on samples of cotton gin 

byproducts stored frozen for >4 months [40% recovery]. 

Cotton Field Trials (860. 1500) 

48156901.der.docx 

Page 3of9 
Aldicarb DCI Residue Chemistry Review DPll 425 180 

Twelve field trials were conducted in the United States during the 2009 growing season in the 

North American Free Trade Agreement (NAFTA) Growing Zones 2 (NC; 1 trial), 4 (AR, MO 

and MS; 3 trials), 6 (TX; I trial), 8 (OK and TX; 4 trials), and l 0 (CA; 3 trials). At each trial 

location, the treated plot received two soil incorporated applications of a 15% granule (GR) 

formulation of aldicarb (TEMIK l 5G). The first application was made at l .2- l .8 lb ai/ A to bare 

soil at planting as a band over the open seed furrow then covered with soil, and the second 

application was made between BBCH 52 (first floral buds visible) and BBCH 61 (beginning of 

flowering) at l .8-2.8 lb ail A as a side dress to a furrow to one side of the plant row then covered 

with soil. The total seasonal application rate was 3.0-4.5 lb ai/A. Retreatment intervals (RTis) 

were 45-102 days. No adjuvants were used. Samples of seed cotton were harvested at a targeted 

preharvest interval (PHI) of 90 days. Additional samples were collected at the OK trial at 

intervals preceding and following the target 90-day PHI, at PH Is of 71, 80, 98, and I 09 days, to 

investigate residue decline. For cotton gin byproducts, samples at six trials were harvested using 

picker or stripper equipment (3 trials each). 

Samples were analyzed for residues of aldicarb, aldicarb sulfone, and aldicarb sulfoxide using 

high performance liquid chromatography with tandem mass spectrometry detection 

(LC/MS/MS), Bayer CropScience Method 0085 l. Residues of the metabolites were determined 

in parent equivalents. The reported limit of quantitation (LOQ; determined as the lowest level of 

method validation, LLMV) was 0.0 I ppm for each analyte in cotton matrices. 

Results 

Following two soil incorporated applications of the 15% GR formulation made at total 

application rates of 3.0-4.6 lb ai/A, combined residues of aldicarb, aldicarb sulfone, and aldicarb 

sulfoxide were <0.03-<0. 139 ppm in/on undelinted cotton seed and <0.03-<0. 197 ppm inion gin 

byproducts. 

In the residue decline trial, maximum combined residues of aldicarb, aldicarb sulfone, and 

aldicarb sulfoxide occurred at the 80-day PHI in both undelinted cotton seed and gin byproducts, 

after which they decreased with increasing PHI in gin byproducts. In seed, residues remained 

relatively stable after the 90-day PHI. 

Samples were stored frozen (- -IO °C) from harvest to extraction for analysis of aldicarb and its 

metabolites aldicarb sulfone and aldicarb sulfoxide for up to 133 days (4.4 months) for 

undelinted cotton seed and I 36 days (4.5 months) for cotton gin byproducts. Samples were 

analyzed within 2 days of extraction. Acceptable storage stability data ( 48156902.der) indicate 

that correction for loss on storage is needed for residues of aldicarb, aldicarb sulfoxide, and 

aldicarb sulfone inion cotton undelinted seed stored frozen for> 15 days (average recovery of 

44% for each analyte for all storage intervals > 15 days) and for residues of aldicarb inion 

samples of cotton gin byproducts stored frozen for >4 months ( 40% recovery). Because residues 

of aldicarb were below the LOQ inion all samples of cotton undelinted seed and gin byproducts, 

the only corrections for loss on storage needed were for quantifiable residues of the metabolites 

inion cotton undelinted seed. Table l summarized the residue values from the cotton tri als, 

corrected for storage losses. 

Page 4 of9 
Aldicarb DCI Residue Chemistry Review DP# 425 180 

Table 1. Summary of Residues from Cotton Field Trials with Aldicarb. 

Crop Matrix Total Application PHI n' Combined Residues2 (ppm parent equivalents) 

Rate (days) Min.3 Max.

3 LAFT-' HAFT-' Median• Mean4 so• 

(lb ai/A) 

Cotton 3.01-4.55 87-11 7 12 <0.03 <0. 199 <0.03 <0.139 O.Q3 0.0453 0.0321 

undelinted seed 

Cotton 3.63-4.55 87-11 7 6 <0.03 <0.226 

gin byproducts 

1 n = number of field trials. 2 Combined residues of aldicarb, aldicarb sulfone. and aldicarb sulfoxide. 3 Values based on total number of samples. 

<0.03 <0.197 0.0502 0.0819 0.0677 

4 Values based on per-trial averages. LAFT = lowest average field trial. HAFT = highest average field trial, SD= standard 

deviation. For computation of the LAFT, I !AFT, median. mean. and standard deviation. values < LOQ arc assumed lo be at the 

LOQ (0.0 I ppm). 

Conclusions 

HED concludes that the submitted cotton studies adequately address the previously identified 

data gaps. Analysis of the results of the 12 new cotton trials ( 4815690 l.der) using the 

Organisation for Economic Co-operation and Development (OECO) tolerance calculation 

procedures results in a suggested tolerance of 0.2 and 0.4 ppm for cotton seed and gin 

byproducts, respectively (Appendix A and B). 

Meat, Milk, Poultry. and Eggs (MMPE) (860.1480) 

The most recent evaluation of aldicarb residues in MMPE commodities was provided in support 

of the Registration Eligibility Decision (RED) (D266396, C. Swartz, 6/2/2000), where HED 

concluded that residues in livestock commodities are classified under 40 CFR § l80.6(a)(3), i. e., 

there is no reasonable expectation of finite residues. Because the submitted cotton field trial 

data show detectable residues in cotton commodities, and these commodities may be fed to 

livestock, an update to the previous determination regarding livestock commodities is needed. 

In a metabolism study (MRID No. 00159570) in which goats were dosed with 14

C-aldicarb for 

I 0 days at 2.5 ppm, radioactive residues were as follows, with the residues of concern (i.e. , 

carbamate metabolites) given in parentheses [aldicarb per se was not detected in milk or tissues]: 

Milk (day I 0): 

Liver: 

Kidney: 

Fat: 

Muscle: 

0.12 ppm (0.0002 ppm) 

0.52 ppm (0.00 I 4 ppm) 

0.1 9 ppm (0.0006 ppm) 

0.02-0.03 ppm (not detected) 

0.08 ppm (0.0002 ppm) 

In a poultry metabolism study, hens were dosed with non-radiolabeled aldicarb and aldicarb 

sulfone for 7 days, followed by 2 1 days of dosing with radiolabeled aldicarb and aldicarb sulfone 

al 0.1, I and 20 ppm in the diet. No residues of concern were identified in either egg whites or 

yolks; following 20 ppm dosing, aldicarb sulfoxide was identified at 0.003 ppm in liver, and no 

other residues of concern were identified in li ver or other tissues. Table 2 summarizes the tissueto-feed ratios determined from the goat and hen metabolism studies. 

Page 5of9 
Aldicarb DCI Residue Chemistry Review DP# 425180 

Table 2. Summary of Coat and Hen Metabolism Studies with Aldicarb. 

Commodity Feeding Level, ppm Residue in Tissue, ppm1 Tissue-to-Feed Ratio 

Milk 2.5 0.0002 0.00008 

Muscle (ruminant) 2.5 0.0002 0.00008 

Fat (ruminant) 2.5 ND .. 

Liver (ruminant) 2.5 0.00 14 0.00056 

Kidney (ruminant) 2.5 0.0006 0.00024 

Eggs 20 ND .. 

Muscle (poultry) 20 ND .. 

Fat (poultry) 20 ND .. 

Liver (poultry) 20 0.003 0.00015 

Skin/Fat (poultry) 20 ND .. 1 Maximum residue. 

In addition to cotton, some rotational crop RACs may be fed to livestock. Previous reviews of 

rotational crop studies have concluded that detectable residues may occur in rotational wheat and 

barley (D200435, J. Garbus, 3/20/ 1995) feedstuffs. Specifically, maximum residues of 0.88 and 

0.60 ppm were found in rotational wheat forage and barley forage, respectively. Although no 

hay data were provided, maximum residues may be estimated from the forage data by correcting 

for dry matter. Thus, wheat hay: 0.88 ppm * (88/25) = 3. l ppm and barley hay: 0.60 ppm * 

(88/30) = 1.8 ppm. Using these values, livestock dietary burdens are estimated as shown in 

Table 3. 

Table 3. Aldicarb Dietary Burdens fo r Livestock. 

More Balanced Diet (MBD) 

Crop Commodity Type 

Residue % DM % Diet Dietary Contribution 

ppm I input ppm 

Beef Cattle 

Wheat1 llay R 3. 1 HAFT 88 15 0.53 

Cotton Meal PC 0.03 Median 89 5 0.002 

Untreated feed NA NA NA NA NA 80 0 

Total NA NA NA NA NA 100 0.53 

Dairy Cattle 

Whcat1 llay R 3.1 HAFT 88 20 0.70 

Whcat1 Forage R 0.88 HAFT 25 20 0.70 

Barley1 llay R 1.8 HAFT 88 5 0. 10 

Cotton Undelinted seed PC 0.03 Median 88 10 0.003 

Untreated feed NA NA NA NA NA 45 0 

Total NA NA NA NA NA 100 1.5 1 

Poultry 

Cotton Meal PC 0.03 Median 89 20 0.006 

Untreated feed NA NA NA NA NA 80 0 

Total NA NA NA NA NA 100 0.006 

Swine 

Cotton Meal PC O.Q3 Median 89 15 0.005 

Untreated feed NA NA NA NA NA 85 0 

Total NA NA NA NA NA 100 0.005 

Rotational crop. 

Page 6of9 
Aldicarb OCI Residue Chemistry Review DP# 425 180 

The maximum residue levels expected in livestock commodities are estimated as a product of the 

appropriate tissue-to-feed ratios and dietary burdens as shown in Table 4. 

T able 4. Estima tion of Secondary Residues from Use o f A ld icarb. 

Commodity T issue-to-Feed Ra tio Die tary Burden (oom) Ex pected Resid ue (ppm) 

Milk 0.00008 1.5 0.00012 

Muscle (cattle) 0.00008 1.5 0.000 12 

Fat (cattle) -- 1.5 -- Liver (cattle) 0.00056 1.5 0.00084 

Kidney (caule) 0.00024 1.5 0.00036 

Eggs -- 0.006 -- Muscle (oouhrv) -- 0.006 -- f at (poultry) -- 0.006 -- Liver (poultry) 0.00015 0.006 0.0000009 

Skin/fat (oouhry) -- 0.006 --

Conclusions 

HED concludes that 40 CFR § l 80.6(a)(3) still applies to all MMPE commodities since the 

maximum expected residues are < 0.00 I ppm [LOQ/1 O]. 

Attachments 

48 156901.der.docx [cotton field trials] 

48156902.der.docx [cotton storage stability] 

481 56903.der.docx [analytical method] 

Page 7 of9 
Aldicarb OCI Residue Chemistry Review 

Appendix A. OECD Tolerance Calcul ations for Aldicarb/Cotton Seed. 

Aldicarb 

Cotton Seed 

USA 

3.5 lb ai/ A, 90-day PHI 

Total nwnber o f data (n ) 

Percentage of censored data 

Nwnber of non- censored data 

Lowest residue 

Highes t residue 

Median resi due 

Me an 

Stand a rd devia tion (SD) 

Cor rec tion factor for censoring (CF) 

Propos ed MRL estimate 

- Highest r esidue 

- Mean + 4 SD 

- CF x 3 Mean 

Unrounded MRL 

Rounded MRL 

High uncertainty of MRL estimate . 

[High level of censoring] 

Re s idues (mg/kg) n 

< 0 . 03 8 

0.0422 1 

0.0538 1 

0.0678 1 

0 . 139 1 

Page 8of9 

12 

67% 

4 

0 . 030 

0 .139 

0 . 030 

0.045 

0 . 032 

0 . 556 

0 . 139 

0 . 173 

0 . 075 

0 .173 

0 . 2 

OP# 425 180 
Aldicarb DCI Residue Chemistry Review 

Appendix B. OECD Tolerance Calculations for Aldicarb/Cotton Gin Byproducts. 

Aldicarb 

Cotton Gin Bypd 

USA 

3.5 lb ai/ A, 90-day PHI 

Total nwnber of data (n) 

Percentage of censored data 

Nwnber 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 

High uncertainty o f MRL e s tima te . 

(Small d a tas et) 

Residues (mg / kg) n 

< 0.03 1 

0.0334 1 

0 . 0413 1 

0. 0 592 1 

0 . 13 1 

0. 1 97 1 

Page 9of9 

6 

17%" 

5 

0 .03 0 

0.197 

0.050 

0 .082 

0.067 

0.889 

0.197 

0 .3 52 

0.218 

0.352 

0 .4 

DP# 425180 
Aldicarb [PC Code 09830 I ]/Bayer CropScience 

B.7.6 Residues Resulting from Supervised T rials 

(Annex IIA 6.3; Annex IHA 8.3) 

B.7.6.1 Residues in Target Crops 

B.7.6.1.1 Cotton 

Document ID: MRID No. 4815690 I 

Report: Gould, T. and Dallstream, K. (20 l 0) TEM IK l 5G - Magnitude of the 

Residue in/on Cottonseed and Cotton Gin Trash. Report Numbers: 

RAA VX002 and M-385788-01-1. Unpublished study prepared by Bayer 

CropScience. 312 p 

Guidelines: EPA OCSPP Harmonized Test Guideline 860.1500 Crop Field Trials 

(August 1996) 

PMRA Regulatory Directive OIR98-02 - Residue Chemistry Guidelines, 

Section 9 - Crop Field Trials 

PMRA Regulatory Directive DIR2010-05 - Revisions to the Residue 

Chemistry Crop Field Trial Requirements 

OECD Guideline 509 Crop Field Trial (September 2009) 

GLP Compliance: No deviations from regulatory requirements were reported which would 

have an impact on the validity of the study. 

Acceptability: The study is considered scientifically acceptable. The acceptability of this 

study for regulatory purposes is addressed in the forthcoming U.S. EPA 

Residue Chemistry Summary Document, DP# 425180. 

Evaluator: William H. Donovan, Ph.D., Chemist, RABY 

Note: This Data Evaluation Record (DER) was originally prepared under contract by Versar. Inc. (6850 Vcrsar Center. 

Springfi eld. VA 22 151: submitted 3/13/ 15). The DER has been reviewed by HED and revised to reflect current Office of 

Pesticide Programs (OPP) policies. 

EXECUTIVE SUMMARY 

In response to the Residue Chemistry Chapter of the Aldicarb RED (DP# 266396, 6/2/00, C. 

Swartz), Bayer CropScience has submitted field trial data for aldicarb on cotton. Twelve field 

trials were conducted in the United States during the 2009 growing season in the North 

American Free Trade Agreement (NAFTA) Growing Zones 2 (NC; 1 trial), 4 (AR, MO and MS; 

3 trials), 6 (TX; 1 trial), 8 (OK and TX; 4 trials), and I 0 (CA; 3 trials). 

Each trial consisted of one untreated plot and one treated control plot. At each trial location, the 

treated plot received two soil incorporated applications of a 15% granule (GR) formulation of 

aldicarb (TEMIK 15G). The first application was made at 1.26- 1. 79 lb ai/ A ( 1.41-2.0 I kg ai/ha) 

to bare soil at planting as a band over the open seed furrow then covered with soil, and the 

second application was made between BBCH 52 (first floral buds visible) and BBCH 6 1 

(beginning of flowering) at 1.75-2.76 lb ai/A (I .97-3.09 kg ai/ha) as a side dress to a furrow to 

one side of the plant row then covered with soil. The total seasonal application rate was 3.01-

4.55 lb ai/A (3.38-5.10 kg ai/ha). Retreatment intervals (RTis) were 45-102 days. No adjuvants 

EPA MRID #: 4815690 1 

PMRA #: NA 

Page I of 11 
Aldicarb [PC Code 09830 I ]!Bayer CropScience 

were used. Samples of seed cotton were harvested at preharvest intervals (PH Is) of 87-117 days. 

Additional samples were collected at the OK trial at intervals preceding and following the target 

90-day PHI, at PHJs of 71 , 80, 98, and 109 days, to investigate residue decline. To produce the 

required samples of cotton gin byproducts, samples at six trials were harvested using picker or 

stripper equipment (3 trials each); samples from the remaining trials were harvested by hand. All 

samples were transported from the field sites to GLP Technologies (Navasota, TX) for 

generation of undelinted cotton seed (all trials) and gin byproducts (six trials). Cotton was 

ginned within 36-92 days of harvest. 

Samples were either shipped under ambient conditions within 1 day of harvest to the ginning 

faci lity, where they were placed in frozen storage, or were maintained frozen at the testing 

facility and shipped frozen to the ginning faci lity. All samples were shipped frozen to the 

analytical laboratory, where they were stored frozen until analysis. The storage intervals for 

samples between harvest and extraction were 67-133 days (2.2-4.4 months) for undelinted cotton 

seed and 69-136 days (2.3-4.5 months) for cotton gin byproducts. Samples were analyzed within 

2 days of extraction. Acceptable storage stability data have been submitted (refer to MRlD 

48156902; B.7.6.2) investigating the stability of residues of aldicarb, aldicarb sulfone, and 

aldicarb sulfoxide in/on cotton undelinted seed and gin byproducts during frozen storage for up 5 

months. The data indicate that residues of all three analytes were unstable inion cotton 

undelinted seed at storage intervals > 15 days. In cotton gin byproducts, residues of aldicarb 

were stable for up to 4 months but declined by the 5-month storage interval, while residues of 

aldicarb sulfoxide and aldicarb sulfone were stable for up to 5 months. The submitted storage 

stability data indicate that correction for loss on storage is needed for residues of aldicarb, 

aldicarb sulfoxide, and aldicarb sulfone inion cotton undelinted seed stored frozen for > 15 days 

(average recovery of 44% for each analyte for all storage intervals > 15 days) and for residues of 

aldicarb in/on samples of cotton gin byproducts stored frozen for >4 months (40% recovery). 

We note that, because residues of aldicarb were below the LOQ in/on all san1ples of cotton 

undelinted seed and gin byproducts in the current study, the only corrections for loss on storage 

needed were for quantifiable residues of the metabolites in/on cotton undelinted seed. 

Samples were analyzed for residues of aldicarb, aldicarb sulfone, and aldicarb sulfoxide using 

high performance liquid chromatography with tandem mass spectrometry detection 

(LC/MS/MS), Bayer CropScience Method 0085 1 with minor modifications. Residues of the 

metabolites were determined in parent equivalents by use of analytical standard solutions 

prepared in parent equivalents. Acceptable method validation and concurrent recoveries were 

reported for samples of cotton undelinted seed fortified with each analyte at 0.01-0. l 0 ppm and 

gin byproducts fortified with each analyte at 0.01-0.40 ppm, thus validating the method. The 

reported limit of quantitation (LOQ; determined as the lowest level of method validation, 

LLMV) was 0.01 ppm for each analyte in cotton matrices. The fortification levels used in 

method validation and concurrent method recovery were adequate to bracket expected residue 

levels (within an order of magnitude for undelinted seed). Concurrent recoveries were corrected 

for apparent residues in controls if present. Residues in treated samples were not corrected for 

residues in controls. 

Following two soil incorporated applications of the 15% GR formulation made at total 

application rates of 3.01 -4.55 lb ai/A (3.38-5. l 0 kg ai/ha), combined residues of aldicarb, 

EPA MRID #: 48156901 

PMRA II: NA 

Page 2 of 11 
Aldicarb [PC Code 09830 I ]/Bayer CropScience 

aldicarb sulfone, and aldicarb sulfoxide (and per-trial averages) were <0.03-<0.199 (<0.03-

<0.1 39) ppm in/on undelinted cotton seed and <0.03-<0.226 (<0.03-<0.197) ppm in/on gin 

byproducts. 

In the residue decline trial, maximum combined residues of aldicarb, aldicarb sulfone, and 

aldicarb sulfoxide occurred at the 80-day PHI in both undelinted cotton seed and gin byproducts, 

after which they decreased with increasing PHI in gin byproducts. In seed, residues remained 

relatively stable after the 90-day PHI. 

I. MATERIALS AND METHODS 

A. MA TE RIALS 

Table B.7.6.1.1-1. Nome nclature fo r Aldicarb and its Metabolites of In terest. 

Common name 

Identity 

CAS no. 

Company experimental name 

Other synonyms (if applicable) 

Metabolite 

Ident ity 

CAS no. 

Company experimental name 

Other synonyms (if a pplicable) 

Metabolite 

Identity 

CAS no. 

Company experimental name 

Other synonyms (if applicable) 

EPA MRID #: 48156901 

PMRA #: NA 

/\ldicarb 

2-Mcthyl-2-(methylthio)propionaldchydc 0-(methyl carbamoyl) oxime 

11 6-06-3 

NA 

NA 

CH3 0 

I 11 /H 

CHrS·C-CH = N-0-C-N 

I ' CH3 CH3 

/\ldicarb sul foxide 

2-Mcthyl-2-(methylsulfinyl)propionaldchyde 0 -(methyl carbamoyl) oxime 

1646-87-3 

NA 

NA 

0 CH3 0 

II I II 

CH3S-C-CH =N- OCNHCH3 

I 

CH3 

Aldicarb sulfone 

2-Mcthyl-2-(rncthylsulfonyl)propionnldehyde 0-(mcthyl carbamoyl) oxirne 

1646-88-4 

NA 

NA 

H3C\ #0 

N CH3 - C 

I \ I 

H 0-N= CH-C-CH:i 

I 

O=S= O 

I 

CH3 

Page 3 of 11 
Aldicarb [PC Code 09830 I ]!Bayer CropScicncc 

B. Study Design 

1. Test Procedure 

Twelve residue trials on cotton were conducted with a 15% GR formulation of aldicarb (TEM IK 

I SG) during the 2009 growing season. Field trial locations by NAFTA growing zone are 

summarized in Table 8.7.6.1.1-2. 

The trials separated by <20 miles have been assessed for independence as detailed in the table 

below. HED has determined that there are sufficient differences between the trials that they may 

be considered separate. 

Independent Trial Determination 1 

Trial Nos. Differenci.:s Decision 

J\ YO I 0-0911A and Location: Sanger, CA vs. r=resno. CA Independent 

AVOl l-09HA Variety: PHY 725 RF (J\CALA) is a Genuity~ Roundup Read)!® Flex conversion of 

PHY 72 vs. Pl IY 755 WRF (ACALA) is a WidcStrike® Insect Protection and Genuit-Y® 

Roundup Readyi> Flex conversion of PHY 72. Both have semi-smooth leaf type. 

medium tall plant height, very good seeding vigor. and high yield potential with 

adaptation across San Joaquin Valley. 

Timing: 20-day offset in planting/first soil application and 7-day offset in harvest 

Soil type: Sandy loam vs. loamy sand (Note: Use pattern is two soil applica1ions. lirst 

application made to bare soil at planting and the second is made as a side dress to the 

furrow to one side of the plant row.) 

•No other dilTerenccs found in criteria. but note that PFI and testing faci lity are different 

for each trial: Carl E. Joplin of Syn Tech Research Inc. for A YO I 0-09HA and Brian D. 

Lange of Euro!ins Agroscience Services for A YO I 1-09HA 1 All assessments arc based on the replicate trial guidance presented in drafi memo 568_ Critcria for Independence of Trials 

04/23/2013 (EPA and PMRA). A separate tank mix was used for all applications. 

Table B.7.6. l.l-2. Trial Numbers and Geographical Locations. 

Crop No. NJ\FT A Growing Zone 

Total Trials I 2 3 4 5 6 7 8 9 10 11 12 

Cotton Sub. I 3 I 4 3 12 

Req.1 Ill 3/2 I/I 4/3 3/2 12/9 

1 As per Table 5 of 860.1500 for cotton. TI1c second number rcOects a 25% reduction 111 the number of trials allowed for the 

crop as a representative commodity in support of a crop group/subgroup tolerance or when application results in no quantifiable 

residues. Per OCSPP 860.1000 Supplement (6/30/08), cotton must be harvested by commercial equipment 10 provide an 

adequate representation of plant residue for the ginning process. Three field trials for harvesting of stripper collon are needed. 

No data arc needed fo r picker collon. 

Locations and detailed use patterns for the trials are provided in Table B. 7.6. l.1-3. 

Table B.7.6. 1.1-3. Study Use Pattern. 

Location: City, End-use 

State: Year Product1 

(Trial ID) 

Sunbury. NC; 15%GR 

2009 

(A YOO l-09HA) 

EPA MR1D #: 48156901 

PMRA #: NA 

Method of Application: 

Timing of J\pplication 

I. Soil incorporated, 

banded to seed furrow: 

at planting, 13BCI I 0 

2. Soil incorporated, 

side dress: B13CH 55 

Yolume2 Rate per 

(gal/A) Application 

[Uha) {lb ai/A) 

[kg ai/ha] 

NIA 1.794 

12.009] 

NIA 2.757 

[3.088] 

Rctreatmcnt Total Surfactant/ Harvest 

Interval Rate Adjuvant Procedures 

(days) (lb ai/A) 

(kg ai/ha] 

-- 4.551 None Picker 

[5.097( 

59 

Page 4 of 11 
Aldicarb [PC Code 09830 I )/Bayer CropScience 

Table B.7.6.1.1-3. Study Use Pattern. 

Location: City. End-use 

State: Year Product 1 

(Trial 10) 

Proctor. AR: 15% GR 

2009 

(A V002-09HA) 

Fisk. MO: 2009 15%GR 

(A V003-09HA) 

Greenvi lle. MS: 15% GR 

2009 

(A V004-091 IA) 

East Bernard. 15% GR 

TX: 2009 

(A V005-09HA) 

Uvalde. TX: 15%GR 

2009 

(A V006-09HA) 

I linton. OK; 15%GR 

2009 

(A V007-09DA) 

Levelland. TX: 15% GR 

2009 

(A V008-09HA) 

Wolfforth, TX; 15%GR 

2009 

(A V009-09HA) 

Sanger. CA; 15%GR 

2009 

(A VO I 0-09HA) 

Fresno. CA: 15%GR 

2009 

(AV0 11-09HA) 

EPA MRID #: 48156901 

PMRA #: NA 

Method of Application: 

Timing of Application 

1. Soil incorporated. 

banded to seed furrow; 

at planting, 13BCH 0 

2. Soil incorporated, 

side dress: BBCH 59 

I. Soil incorporated. 

banded to seed furrow; 

at planting. Bl3CH 0 

2. Soil incorporated. 

side dress; OBCH 55 

I. Soil incorporated, 

banded to sced furrow: 

at planting. BBCH 0 

2. Soil incorporated. 

side dress: BBCI I 59 

I. Soil incorporated. 

banded to seed furrow; 

at planting. BBCH 0 

2. Soil incorporated. 

side dress; Bl3CH 60 

I. Soil incorporated, 

banded to seed furrow; 

at planting, BBCH 0 

2. Soil incorporated. 

side dress; OBCI I 52 

I . Soil incorporated. 

banded to seed furrow; 

at planting. BBCH 0 

2. Soil inco rporated. 

side dress; BBCI I 60 

I. Soil incorporated. 

banded to seed furrow; 

at planting, BBCH 0 

2. Soil incorporated. 

side dress; BBC! I 60 

I. Soil incorporated, 

banded to seed furrow; 

at planting, BBCH 0 

2. Soil incorporated, 

side dress; OBCH 60 

I. Soil incorporated. 

banded to seed furrow: 

at planting. BBCH 0 

2. Soil incorporated. 

side dress; BBCI I 60 

I. Soil incorporated. 

banded to seed furrow: 

at planting, BBCH 0 

2. Soil incorporated, 

side dress: OBCI I 61 

Volume2 

(gal/A) 

[Uha] 

NIA 

NIA 

NIA 

NIA 

NIA 

NIA 

NIA 

NIA 

NIA 

NIA 

NIA 

NIA 

NIA 

IA 

NIA 

NIA 

NIA 

NIA 

NIA 

NIA 

Rate per Retreatment Total Surfactant/ Harvest 

Application Interval Rate Adjuvant Procedures 

(lb ai/A) (days) (lb ail A) 

[kg ai/ha j [kg ai/ha] 

1.520 -- 3.680 None Picker 

[I. 7041 [4.125] 

2. 160 45 

[2.421] 

1.551 -- 3.665 None Picker 

[I. 739] 14.108] 

2. 114 68 

[2.370] 

1.530 -- 3.620 None Hand 

[1.715] [4.058] picked 

2.090 46 

[2.343] 

1.570 -- 3.630 None Stripper 

r 1.1601 [4.069] 

2.060 5 1 

[2.309] 

1.591 -- 3.691 None Stripper 

(1.784] [4. 138] 

2. 100 60 

[2.354] 

1.762 -- 4. 150 None Stripper 

I 1.975] [4.652] 

2.388 69 

[2.677] 

1.505 -- 3.604 None I land 

[ 1.687] [4.040] picked 

2.099 61 

[2.353] 

1.473 -- 3.572 None Hand 

[1.65 1] 14.005] picked 

2.099 56 

[2.353] 

1.429 -- 3.579 None Hand 

[ 1.602] [4.012] picked 

2. 150 70 

[2.411] 

1.504 -- 3.600 None Hand 

[ 1.686) [4.036] picked 

2.096 55 

[2.350] 

Page 5 of I I 
Aldicarb [PC Code 09830 I ]/Bayer CropScicnce 

Table 8.7.6.1.1-3. Study Use Pattern. 

Location: City, End-use Method of Application; Volume2 Rate per Retreatment Total Surfactant/ Harvest 

State: Year Product' Timing of Application (gal/A) Application Interval Rate Adjuvant Procedures 

(Trial 10) [L/ha] (lb ai/A) (days) (lb ail/\) 

[kg ailha] [kg ai/ha] 

Blythe, CA: 15%GR I. Soil incorporated, NIA 1.260 -- 3.013 None Hand 

2009 banded lo seed furrow; (1.41 2] [3 .378] picked 

(A VO l 2-09HA) at planting. BBCH 0 

2. Soil incorporated. NIA 1.753 102 

side dress; Bl3CI I 55 [1 .965] 1 15% granule (GR) formulation (TEMIK I 5G). 2 Spray volume is not applicable (N/A) for granule application. 

Cotton was grown and maintained according to typical agricultural practi ces. Irrigation was used 

to supplement rainfall as needed. No unusual weather conditions were reported to have 

adversely affected crop production or yield during the study. 

Sample Handling and Preparation 

Single control and duplicate treated samples of seed cotton were harvested at PHis of 87-117 

days. Additional samples were collected at the OK trial at intervals preceding and following the 

target 90-day PHI, at PHis of 71 , 80, 98, and 109 days, to investigate residue decline. To 

produce the required samples of cotton gin byproducts, samples at six trials were harvested using 

picker or stripper equipment (3 trials each); samples from the remaining trials were harvested by 

hand. Sample sizes were 34 lb for stripper harvest, 45 lb for picker harvest, and l kg for 

manual collection. All samples of seed cotton were shipped to OLP Technologies (Navasota, 

TX) for generation of cotton undelinted seed and gin byproducts. Samples from Trials A YOO I 

and A V006 were shipped under ambient conditions within 1 day of harvest by the field 

cooperator or courier; samples from the remaining trials were placed in frozen storage at the field 

sites within ~ 7 .5 hours of harvest and were shipped via freezer truck to OLP Technologies. At 

OLP Technologies, samples were stored frozen (<-5 °C) prior to and following generation of 

cotton undelinted seed and gin byproducts. San1ples of seed cotton were cleaned with a stick 

extractor to remove gin byproducts within 36-92 days of harvest. Samples were shipped frozen 

4-27 days after ginning to the analytical laboratory, Pyxant Labs (Colorado Springs, CO) for 

homogenization, extraction, and analysis, except for samples from Trial A V005, which were 

shipped first to Bayer Research Park (BRP; Stillwell, KS) and then sent to Pyxant Labs. At 

Pyx ant Labs, samples were maintained frozen ( <-1 0 °C) prior to processing and analysis. In 

preparation for analysis, samples were homogenized in the presence of dry ice. 

2. Description of Analytical Procedures 

Samples were analyzed for residues of aldicarb, aldicarb sulfoxide, and aldicarb sul fone using 

LC/MS/MS, Bayer CropScience Method 0085 J with minor modifications. Modifications 

included the following: minor procedural, materials, and instrument changes; removal of 

reserpine as an internal standard; optimization of instrument parameters and gradient; and 

monitoring a different ion transition for quantitation of aldicarb sulfone to improve sensitivity. 

A complete description (including method validation data) of this method is provided in a 

separate file (refer to 48156903.der.docx). This method was also used for data collection in the 

storage stability study (refer to 481 56902.der.docx). 

EPA MR1D #: 48156901 

PMRA #: NA 

Page 6of11 
Aldicarb [PC Code 098301 ]/Bayer CropScicnce 

Briefly, samples were extracted twice with dichloromethane (DCM):acetone (75:25, v:v) and 

filtered. The extracts were combined and diluted with DCM/acetone. Ethylene glycol was 

added, and the mixture was concentrated, reconstituted in acetonitril e, and diluted buffer 

(ammonium acetate and acetic acid diluted with water), and filtered. The filtrate was re-diluted 

with buffer for LC/MS/MS analysis. Residues of the metabolites were determined in parent 

equivalents by use of analytical standard solutions prepared in parent equivalents. 

The reported LOQ (determined as the LLMV) was 0.0 I ppm for each analyte in cotton matrices. 

We note that the petitioner also presented calculated values for the LOO based on the recoveries 

obtained from samples Fortified with each analyte at the 0.0 I-ppm fortification level. The LOD 

was calculated by multiplying the standard deviation of recovery measurements at the LLMV by 

the one-tailed t-statistic at the 99% confidence level for seven replicates and adding this to the 

average residue found in the untreated control. The calculated LODs for aldicarb, aldicarb 

sulfone, and aldicarb sulfoxide were 0.0040, 0.0054, and 0.0055 ppm, respecti vely, in/on 

undelinted cotton seed and 0.0034, 0.0053, and 0.0037 ppm, respectively, inion cotton gin 

byproducts. 

II. RES UL TS AND DISCUSSION 

Method performance was evaluated during method validation and by use of concurrent recovery 

samples. For method validation, samples of undelinted cotton seed and gin byproducts were 

fortified with aldicarb, aldicarb sulfone, and aldicarb sulfoxide at 0.01 , 0. 10 (undelinted seed 

only), and 0.40 ppm (gin byproducts only). For concurrent recovery, samples were fortified with 

aldicarb, aldicarb sulfone, and a ldicarb sulfoxide at 0.0 1 ppm for undelinted cotton seed and at 

0.0 I and 0.20 ppm for cotton gin byproducts. Recoveries were generall y within the acceptable 

range of 70-120%; therefore, the method was considered valid for the analysis of aldicarb, 

aldicarb sulfone, and aldicarb sulfoxide residues in cotton matrices (Table B.7.6.1.1-4). The 

fortification levels bracketed the measured residues (within an order of magnitude for undelinted 

seed). Concurrent recoveries were corrected for apparent residues in controls if present. 

The detector response was linear for aldicarb, aldicarb sulfoxide, and aldicarb sulfone 

(coefficient of detennination, r2 ::;:0.9982) within the range of 5-1000 ng/g. Representative 

chromatograms of control samples, fortified samples, and treated samples were provided. The 

control chromatograms generally had no peaks of interest above the chromatographic 

background. The fortifi ed sample chromatograms contained only the analyte of interest, and 

peaks were symmetrical and well defined. Apparent residues in controls were below the LOQ 

( <0.01 ppm) for both matrices. The reported residue values were not corrected for apparent 

residues in controls. Residues of the metabolites were detennined in parent equivalents by use of 

analytical standard solutions prepared in parent equivalents. 

EPA MRJD #: 4815690 1 

PMRA #: NA 

Page 7of 11 
Aldicarb (PC Code 09830 I ]/Bayer CropScience 

Table B.7.6.1.1-4. Summary of Method Validation a nd Procedural/Concurrent Recoveries of Aldicarb, 

Aldicarb Sulfo ne, a nd Ald icarb Sulfoxide from Cotton Matrices. 

Matrix Analyte Fonification Sample size Rccovcries1 Mean ± Std. Dev. 

Level (ppm) (n) (%) (%) 

Method vnlid ntion 

Undelinted seed Aldicarb 0.0 I 0-0. 100 10 72-106 9 1± 11 

Aldicarb sulfone 0.010-0.100 10 75-1 06: 121 93 ± 14 

Aldicarb sulfoxide 0.010-0.100 10 56: 73-104 83 ± 15 

Gin byproducts Aldicarb 0.0 I 0-0.400 10 75-112 92 ± 13 

Aldicarb sulfone 0.0 I 0-0.400 10 72-120 95 ± 12 

Aldicarb sulfoxide 0.010-0.400 10 66: 70-1 00 83 ± 11 

Concurrent recoveries 

Undclintcd seed Aldicarb 0.010 18 79-98 92 ± 5.4 

Aldicarb sulfonc 0.010 18 75-101 88 ± 7.8 

Aldicarb sulfoxidc 0.010 18 70-93 80 ± 6.0 

Gin byproducts Aldicarb 0.010-0.200 7 80-100 90 ± 8.9 

Aldicarb sulfone 0.0 I 0-0.200 7 74-103 91± 11 

Aldicarb sulfoxide 0.0 I 0-0.200 7 72-1 00 87 ± 9.8 1 Concurrent recoveries were corrected for apparent residues in controls. 

Samples were stored frozen (- -JO °C) from harvest to extraction for analysis of aldicarb and its 

metabolites aldicarb sulfone and aldicarb sulfoxide for up to 133 days (4.4 months) for 

undelinted cotton seed and 136 days ( 4.5 months) for cotton gin byproducts (Table 8. 7 .6.1.1-5). 

Samples were analyzed within 2 days of extraction. Acceptable storage stability data have been 

submitted (refer to MRID 48156902) investigating the stability of residues of aldicarb, aldicarb 

sulfone, and aldicarb sulfoxide in/on cotton undelinted seed and gin byproducts during frozen 

storage for up 5 months. The data indicate that residues of all three analytes were unstabl e in/on 

cotton undelinted seed at storage intervals > 15 days. In cotton gin byproducts, residues of 

aldicarb were stable for up to 4 months but declined by the 5-month storage interval, while 

residues of aldicarb sulfoxide and aldicarb sulfone were stable for at least 5 months. The 

submitted storage stability data indi cate that correction for loss on storage is needed for residues 

of aldicarb, aldicarb sulfoxide, and aldicarb sulfone in/on cotton undelinted seed stored frozen 

for> 15 days (average recovery of 44% for each analyte for all storage intervals > 15 days) and 

for residues of aldicarb in/on samples of cotton gin byproducts stored frozen for >4 months ( 40% 

recovery). We note that, because residues of aldicarb were below the LOQ in/on all samples of 

cotton undelinted seed and gin byproducts, the only corrections for loss on storage needed were 

for quantifiable residues of the metabolites in/on cotton undelinted seed. 

Table B.7.6.1.1-5. Summary of Storage Conditions. 

Matrix Storage Temperature Actual Storage Interval of Demonstrated Storage Stability 

(oC) Duration1 

Collon, undelinted <-5 at GLP 67-133 days Residues ofaldicarb. aldicarb sulfoxide. and aldicarb 

seed Technologies (2.2-4.4 months) sulfonc were unstable during frozen storage in/on cotton 

<-I 0 at Pyxant undelinted seed at storage intervals> 15 days. 2 

Cotton gin 69-136 days Residues of aldicarb were stable during frozen storage 

byproducts (2.3-4.5 months) for up to 4 months but declined by the 5-month storage 

interval; residues of aldicarb sulfoxide and aldicarb 

sulfone were stable for up to 5 months. 2 

1 Interval from harvest to extraction. Samples were analyzed w11hm 0-2 days of extraction. 2 Refer to 48156902.0ER; B.7.6.2 

EPA MRID #: 48156901 

PMRA #: NA 

Page 8 of1 I 
Aldicarb [PC Code 09830 I ]/Bayer CropScience 

The results from the submitted field trials are presented in Tables B.7.6.1.1-6 and B.7.6. 1. 1-7. 

Following two soil incorporated applications of the 15% GR formulation made at total 

application rates of 3.01-4.55 lb ai/A (3.38-5. l 0 kg ai/ha), combined residues of aldicarb, 

aldicarb sulfone, and aldicarb sul foxide (and per-trial averages) were <0.03-<0. 199 ( <0.03-

<0. 139) ppm in/on undelinted cotton seed and <0.03-<0.226 (<0.03-<0. 197) ppm in/on gin 

byproducts. 

In the residue decline trial, maximum combined residues of aldicarb, aldicarb sulfone, and 

aldicarb sulfoxide occurred at the 80-day PHI in both undelinted cotton seed and gin byproducts, 

after which they decreased with increasing PHI in gin byproducts. In seed, residues remai ned 

re latively stable after the 90-day PHL 

Table B.7.6. 1.1-6. Residue Da ta from Cotton Fie ld Tria ls with Aldicarb. 1 

Location: City, Zone Co11on/ 

State: Year Variety 

(Trial ID) [Harvest Eq.] 

Sunbury. NC: 2 DPL 445 BR 

2009 [Picker] 

(A VOO 1-091-lA) 

Proctor, AR; 4 PHY375WRF 

2009 [Picker] 

(A V002-09H/\) 

Fisk. MO: 2009 4 DP 164 B2RF 

(A V003-09HA) [Picker] 

Greenville. MS: 4 Delta Pinc 

2009 0935 BGll/Rf 

(A V004-09HA) 

East Bernard. 6 DP0924 B2F 

TX: 2009 [Stripper] 

(A V005-09HA) 

Uvalde, TX: 8 DP 16 1 B2RF 

2009 [Stripper) 

(A V006-091 I/\) 

EPA MRID #: 48156901 

PMRA #: NA 

Matrix Rate Pl-11 2 

(lb ai/A) (days) 

(kg 

ai/ha] 

Seed. 4.551 117 

undelintcd [5.0971 

Gin 

byproducts 

Seed, 3.680 90 

undelinted [4.125) 

Gin 

byproducts 

Seed. 3.665 97 

undc lintcd [4. 108) 

Gin 

byproducts 

Seed. 3.620 97 

undclinted [4 .058] 

Seed. 3.630 89 

undelintcd [4.0691 

Gin 

byproducts 

Seed. 3.69 1 87 

undelintcd [4. 138] 

Gin 

byproducts 

Residues3 (ppm parent equivalents) [Average! 

Aldicarb Aldicarb Aldicarb Combine5 

Sulfone4 Sulfoxide4 

D, ND, ND, <0.03, 

ND ND ND <0.03 

[<0.0 1] [<O.O IJ [<0.0 1] [<0.03] 

ND. ND. ND. <0.03, 

ND ND ND <0.03 

l<0.0 1] [<0.01] [<O.O IJ [<0.03] 

ND. ND, ND, <0.03, 

D ND ND <0.03 

1<0.0 1] [<0.0 1] [<0.0 1] [<0.031 

ND, 0. 104. 0.0407. <0. 155. 

ND 0.0649 0.0305 <0. 105 

[<0.0 1] [0.08451 [0.0356] [<0. 130] 

ND. ND, 0.03 18, <0.05 18, 

ND ND 0.0639 <0.0839 

1<0.0 11 [<0.0 1) [0.0478] f <0.0678) 

ND. (0.00684), 0.0408. <0.0608, 

ND (0.00802) 0.0376 <0.0576 

[<0.01) [<0.0 1] [0.0392] [<0.0592) 

ND, ND. (0.00946). <0.03, 

ND ND (0.00554) <0.03 

[<0.0 1] [<0.0 I] [<0.0 1) [<0.03] 

ND. ND. ND. <0.03, 

D ND ND <0.03 

l<0.0 1] [<0.0 11 [<0.0 1] [<O.OJJ 

ND, (0.00656), 0.0 150, <0.0350, 

ND ND 0.0 11 7 <0.03 17 

1<0.0 1] [<0.0 1] [0.01 34] (<0.0334] 

ND, ND, ND, <0.03, 

ND ND ND <0.03 

[<0.0 1] [<0.0 IJ r<o.o n r<o.031 

ND. (0.007 12), 0.0182, <0.0382. 

ND 0.0120 0.0223 <0.0443 

[<0.01) [<0.01 101 f0.0203) r<o.04 131 

Page 9of11 
Aldicarb [PC Code 09830 I ]/Bayer CropScience 

Table B.7.6.1.1 -6. Residue Data from Cotton Field Trials with Aldicarb. 1 

Location : City. Zone Cotton/ Matrix Rate PHl 2 

State: Year Variety (lb ai/A) (days) 

(Trial ID) (1 larvest Eq. I [kg 

ai/hal 

Hinton. OK; 8 FM 906382F Seed, 4.150 7 1 

2009 [Stripper] undclinted 14.652) 

(A V007-09DA) 

80 

90 

98 

109 

Gin 7 1 

byproducts 

80 

90 

98 

109 

Levelland. TX; 8 fM9063 B2F Seed, 3.604 90 

2009 undclintcd [4.040] 

(A Y008-09HA) 

Wolfforth. TX; 8 327382RF Seed. 3.572 90 

2009 undelinted [4.005] 

(A V009-09HA) 

Sanger, CA: 10 PHY 725 RF Seed, 3.579 88 

2009 (ACALA) undelintcd [4 .012] 

(A VO 10-09!-IA} 

Fresno, CA; 10 PHY 755 Seed. 3.600 90 

2009 WRF Acala undclintcd (4.036] 

(A YO 1 I -0911A) 

Blythe, CA; 10 D&PL 164 Seed. 3.013 89 

2009 B2RF undclinted (3.378) 

(A YO 12-091 IA) 

1 A 15% granule (GR) formulation (TEMIK 150) of a ldicarb was used. 2 The target PHI is balded for the decline trial. 

Residues' (ppm parent equivalents) !Average ! 

Aldicarb Aldicarb Aldicarb Combines 

Sulfonc4 Sulfoxide4 

ND, ND. ND. <0.03. 

ND ND ND <0.03 

[ <0.0 I] [<0.01) [<0.011 [<0.031 

0. 0.0264, 0. 140, <0. 176. 

ND 0.0266 0.1 55 <0. 192 

[<0.0 1) 10.0265) [0. 148] [<0.184] 

ND. ND. 0.0284, <0.0484. 

ND ND 0.0391 <0.0591 

[<0.0ll [<0.01) [0.0338) [<0.0538] 

ND. ND. 0.0441 , <0.0641. 

ND NO 0.0357 <0.0557 

[<0.011 [<0.011 [0.0399) [<0.0599) 

ND. ND. 0.0545, <0.0745. 

ND ND 0.0420 <0.0620 

[<0.0 11 [<0.01] (0.0483] [<0.0683) 

ND. 0.0388, 0.120. <0. 169. 

NO 0.0514 0. 186 <0.247 

[<0.0 1] [0.0451] [0. 153] [<0.208) 

ND. 0.0592, 0.261. <0.330. 

ND 0.0758 0.306 <0.392 

[<0.01] 10.0675) [0.284] [<0.3611 

ND. 0.0247, 0. 134, <0.169. 

D 0.0352 0. 181 <0.226 

[<0.011 [0.03001 [0. 157] [<0. 197] 

ND, 0.0278, 0.148. <0. 186. 

D 0.0283 0. 160 <0. 198 

[<0.01] 10.0280] [0.154] [<0. 1921 

ND, 0.0236, 0.118. <0. 152. 

ND 0.0195 0.1 12 <0. 142 

[<0.01] [0.0215) 10.115] 1<0. 147] 

ND, ND. D. <0.03. 

ND ND ND <0.03 

[<0.0 1] [<0.011 [<0.011 [<0.031 

ND. ND. ND. <0.03. 

ND ND ND <0.03 

[<0.0 1 J f<0.01] [<0.01] [<0.03] 

ND. ND. (0.00683). <0.03. 

ND ND ND <0.03 

[<0.01] [<0.01] [<0.01) l<0.03] 

ND, ND. 0.0595, <0.0795. 

ND 0.0520 0.137 <0.199 

[<0.01] 1<0.03101 10.0983] [<0. 139] 

ND. ND. NO. <0.03, 

ND ND 0.0343 <0.0543 

[<0.0 1] [<0.0 1] [<0.0222) [<0.0422] 

3 NO= Not detected (<LOO). The LODs for aldicarb. aldicarb sulfone. and aldicarb sulfoxide, respectively, were 0.0040. 

0.0054. and 0.0055 ppm for undelinted seed and 0.0034, 0.0053, 0.0037 ppm for gin byproducts. The LOQ was 0.0 I ppm for 

each analyte in both matrices. Values between the LOO and LOQ are reported in parenthesis. Combined residues and per tria l 

averages were calculated by the study reviewer using the LOQ for all residues reported as <LOQ. Residues of the metabolites 

were determined in parent equivalents by use of analytical standard solutions prepared in parent equivalents. 

EPA MRID #: 48 15690 1 

PMRA #:NA 

Page 10of11 
/\ldicarb [PC Code 09830 I ]/Bayer CropScience 

•Quantifiable residues of aldicarb sulfone and aldicarb sulfoxide in/on cotton undelinted seed were corrected for loss on storage 

(calculated as reported residut:/44% recovery) by lhe swdy reviewer and arc highlighted above. 5 Combined residues of aldicarb. a ldicarb sulfone. and aldicarb sulfoxide [which corresponds to the residue definition for 

enforcement purposes!. 

Table B. 7.6.1. 1-7. Summary of Residues from Cotton Fie ld Trials w ith Aldica rb. 

Crop Malrix Total Applicalion Pi ii nl Combined Rcsiducs2 (ppm parent equivalenls) 

Rate (days) Min.

3 Max.3 LAfT" HAFT4 Median4 Mean4 

(lb ai/A) 

(kg ai/ha] 

Cotton 3.013-4.551 87-117 12 <0.03 <0. 199 <0.03 <0. 139 0.03 0.0453 

undelinted seed [3.378-5.0971 

Cotton 3 .630-4.551 87-117 6 <0.03 <0.226 <0.03 <0.197 0.0502 0.08 19 

gin byproducts (4.069-5.097 1 

1 n = number of field trials. 2 Combined residues of aldicarb. aldicarb sulfonc. and aldicarb sulfoxide. 1 Values based on total number of samples. 

SD4 

0.0321 

0.0677 

• Values based on per-trial averages. LAFT = lowest average field trial, I !AFT = highest average field trial, SD= standard 

deviation. ror compulation of the LAFT, I !AFT. median, mean. and standard deviation. values< LOQ arc assumed to be at the 

LOQ (0.01 ppm). 

III. CONCLUSIONS 

The cotton field trials are considered scientifically acceptable. Following two soil incorporated 

applications of the 15% GR formulation made at total application rates of 3.01-4.55 lb ai/A 

(3.38-5.10 kg ai/ha), combined residues of aldicarb, aldicarb sulfone, and aldicarb sulfoxide (and 

per-trial averages) were <0.03-<0.199 (<0.03-<0.1 39) ppm in/on undelinted cotton seed and 

<0.03-<0.226 ( <0.03-<0. 197) ppm in/on gin byproducts. 

Jn the residue decline trial, maximum combined residues of aldicarb, aldicarb sulfone, and 

aldicarb sulfoxide occurred at the 80-day PHI in both undelinted cotton seed and gin byproducts, 

after which they decreased with increasing PH I in gin byproducts. In seed, residues remained 

relatively stable after the 90-day PHI. 

An acceptable method was used for residue quantitation, and adequate storage stability data have 

been submitted to support sample storage durations and conditions for all analytes. Based on the 

results of the storage stability study, quantifiable residues of aldicarb sulfoxide and aldicarb 

sulfone in/on cotton undelinted seed were corrected for loss on storage (calculated as reported 

residue/44% recovery). 

REFERENCES 

DP# 266396, 612100, C. Swartz (Residue Chemistry Chapter of the Aldicarb RED). 

EPA MRID #: 4815690 1 

PMRA #: NA 

Page 11 of 11 
Aldicarb (PC Code 09830 l ]/Bayer CropScience 

B.7.6 Residues Resulting from Supervised Trials 

(Annex IIA 6.3) 

B.7.6.2 Stability of Residues Prior to Analysis 

B.7.6.2.1 Cotton 

Document ID: MRID No. 48156902 

Report: Seal, S. and Gould, T. (2010) Storage Stability of Aldicarb, Aldicarb 

Sulfoxide, and Aldicarb Sulfone on Cottonseed and Cotton Ginned By 

Products. Report Numbers: RAA VPOO 1 and M-385995-01-1. 

Unpublished study prepared by Bayer CropScience. 155 p. 

Guidelines: EPA OCSPP Harmonized Test Guideline 860.1380 Storage Stability Data 

(August 1996) 

PMRA Regulatory Directive DIR98-02 - Residue Chemistry Guidelines, 

Section 5 - Storage Stability Data 

OECD Guideline 506 Stability of Pesticide Residues in Stored 

Commodities (October 2007) 

GLP Compliance: No deviations from regulatory requirements were reported which would 

have an impact on the validity of the study. 

Acceptability: The study is considered scientifically acceptable. The acceptability of this 

study for regulatory purposes is addressed in the forthcoming U.S. EPA 

Residue Chemistry Summary Document, DP# 425 180. 

Evaluator: William H. Donovan, Ph.D., Chemist, RABY 

Note: This Data Evaluation Record (DER) was originally prepared under contract by Vcrsar. Inc. (6850 Versar Center, 

Springfield. VA 2215 1: submitted 3/13/15). The DER has been reviewed by HED and revised to refl ect current Oflice of 

Pesticide Programs (OPP) policies. 

EXECUTIVE SUMMARY 

Bayer CropScience has submitted a storage stability study with aldicarb and its metabolites 

aldicarb sulfoxide and aldicarb sulfone on cotton undelinted seed and gin byproducts. Samples 

of untreated commodities were fortified separately with each analyte at 0.10 ppm, placed in 

frozen storage (S-20 °C), and analyzed at storage intervals of - 0, 1, 1.3 (seed only), 2, 4, and 5 

months (0, 27-28, 38 (seed), 55-56, 120-121 , and 148-152 days). Because decline was observed 

in/on cotton undelinted seed for residues of all three analytes following 1 month of storage, 

additional samples of cotton undelinted seed were prepared midway through the study and were 

analyzed at weekly storage intervals of -0, 1, 2, 3, 4, and 7 weeks (8, 15, 22, 28, and 47 days) to 

more accurately monitor loss on storage. 

Samples were analyzed for residues of aldicarb, aldicarb sulfoxide, and aldicarb sulfone using 

high performance liquid chromatography with tandem mass spectrometry detection 

(LC/MS/MS), Bayer CropScience Method 0085 1 with minor modifications. Acceptable 

concurrent recoveries were reported for samples of cotton undelinted seed and gin byproducts 

fortified with each analyte at 0.10 ppm, thus validating the method. The reported limit of 

EPA MRID #: 48156902 

PMRA #: NA 

Page 1 of10 
Aldicarb [PC Code 09830 I ]/Bayer CropScience 

quantitation (LOQ; determined as the lowest level of method validation, LLMV) was 0.0 I ppm 

for each analyte in cotton matrices. Concurrent recoveries and recoveries in stored samples were 

corrected for apparent residues in controls. 

In the 5-month study for cotton undelinted seed, residues of aldicarb, aldicarb sulfoxide, and 

aldicarb sulfone declined fo llowing I month of frozen storage (recoveries of 31-33%), and 

generally appeared to stabilize at subsequent storage intervals. In the 7-week study for 

undelinted seed, loss on storage was observed for residues of all three analytes at storage 

intervals > 15 days. When the results for both the 5-month and the 7-week studies are combined, 

the average recoveries for residues of aldicarb, aldicarb sulfoxide, and aldicarb sulfone in/on 

cotton undelinted seed at all storage intervals >15 days were 43-46% (overall average recovery 

for all three analytes of - 44%). The data for cotton gin byproducts indicate that residues of 

aldicarb were stable during frozen storage for up to 4 months but declined by the 5-month 

storage interval ( 40% recovery), while residues of aldicarb sulfoxide and aldicarb sulfone were 

stable for up to 5 months. 

The submitted storage stability data indicate that correction for loss on storage is needed for 

residues of aldicarb, aldicarb sulfoxide, and aldicarb sulfone in/on cotton undelinted seed stored 

frozen for > 15 days and for residues of aldicarb in/on samples of cotton gin byproducts stored 

frozen for >4 months. 

I. MATERIALS AND METHODS 

A. MATERIALS 

1. Test Material 

Table B.7.6.2.1-1. Nomenclature fo r Aldicarb a nd its Meta bolites of Interest. 

Common name 

Identity 

CAS no. 

Company experimental name 

Other synonyms (if a1>plicable) 

Metabolite 

Identity 

CAS no. 

Company experimental name 

Other synonyms (if applicable) 

EPA MRJD #: 48156902 

PMRA #: NA 

Aldicarb 

2-Methyl-2-(mcthylthio)propionaldchyde 0-(methyl carbamoyl) ox imc 

11 6-06-3 

NA 

NA 

CH3 0 

I 11 /H 

CHr S·C-CH = N-0-C-N 

I ' CH3 CH3 

Aldicarb sulfoxidc 

2-Mcthyl-2-(methylsulfinyl)propionaldehydc 0-(mcthyl carbamoyl) oxime 

1646-87-3 

NA 

NA 

Page 2 of 10 
Aldicarb [PC Code 09830 l]fBayer CropScience 

Table B.7.6.2. 1-l. Nomenclature for Aldica rb and its Metabolites of Interest. 

0 CH3 0 

II I II 

CH3S-C-CH = N- OCNHCH3 

I 

CH3 

Metabolite Aldicarb sulfone 

Identity 2-Mc1hyl-2-(rnc1hylsulfonyl)propionaldchydc 0-(rncthyl carbarnoyl) oxirnc 

CAS no. 1646-88-4 

Company experimental name NA 

Other synonyms (if applicable) NA 

H3C lo \ 

N CH3 -C 

I \ I 

H 0-N=CH-C- CH:i 

I 

O=S= O 

I 

CH3 

2. Test Commodity 

Matrices: Cotton undelinted seed and gin byproducts 

B. STUDY DESIGN 

I. Test Procedure 

Samples of untreated homogenized cotton undelinted seed and gin byproducts obtained from 

Bayer CropScience were separately fortified with aldicarb, aldicarb sulfoxide, and aldicarb 

sulfone, each at 0.10 ppm, and placed in a freezer where they were stored at S-20 °C from 

fortification until extraction and analysis. 

Day 0 sample sets included nine fortified samples (three replicates for each analyte), and two 

control samples. Analytical sets for each storage interval included two fresh fortification 

samples, two storage stability samples for each analyte, and two control samples. Samples of 

cotton undelinted seed and gin byproducts were analyzed at storage intervals of - 0, 1, 1.3 (seed 

only), 2, 4, and 5 months (0, 27-28, 38 (seed), 55-56, 120-12 1, and 148-152 days). Because 

decline was observed in/on cotton undelinted seed for residues of all three analytes following 1 

month of storage, additional samples of cotton undelinted seed were prepared midway through 

the study and were analyzed at weekly storage intervals of - 0, I, 2, 3, 4, and 7 weeks (8, 15, 22, 

28, and 47 days) to more accurately monitor loss on storage. 

The registrant noted that some of the stock solutions for the metabolites were prepared in parent 

equivalents and some were not. For the cases in which stock solutions were not prepared in 

parent equivalents, results were calculated in parent equivalents by the registrant using molecular 

weight conversion factors. The registrant reported recovered residues for the metabolites both as 

unconverted values and converted to parent equivalents for all storage intervals. Because 

samples were fortified separately with each analyte and because conversion to parent equivalents 

EPA MR.ID #: 48156902 

PMRA #: NA 

Page 3of 10 
Aldicarb [PC Code 09830 !]/Bayer CropScience 

has no impact on recovery values, the recovered residues for metabolites reported herein do not 

reflect conversion lo parent equivalents. 

2. Description of Analytical Procedures 

Samples were analyzed for residues of aldicarb, aldicarb sulfoxide, and aldicarb sulfone using 

LC/MS/MS, Bayer CropScience Method 00851 with minor modifications. Modifications 

included the following: minor procedural, materials, and instrument changes; removal of 

reserpine as an internal standard; optimization of instrument parameters and gradient; and 

monitoring a different ion transition for quantitation of aldicarb sulfone to improve sensitivity. 

A complete description (including method validation data) of this method is provided in a 

separate file (refer to 48156903.der.docx). This method was also used for data collection in the 

cotton crop field trial study (refer to 4815690 l .der.docx). 

Briefly, samples were extracted twice with dichloromethane (DCM):acetone (75:25, v:v) and 

filtered. The extracts were combined and diluted with DCM/acetone. Ethylene glycol was 

added, and the mixture was concentrated, reconstituted in acetonitrile, and diluted buffer 

(ammonium acetate and acetic acid diluted with water), and fi ltered. The filtrate was re-diluted 

with buffer for LC/MS/MS analysis. 

The reported LOQ (determined as the LLMV) was 0.01 ppm for each analyte in each matrix; the 

limit of detection (LOD) was not reported. 

II. RESULTS AND DISCUSSION 

Method performance was evaluated by use of concurrent recovery samples by fortifying 

untreated samples of cotton undelinted seed and gin byproducts with each analyte at 0. 10 ppm. 

Recoveries were within the acceptable range of 70-120%; therefore, the method was considered 

valid for the analysis of aldicarb, aldicarb sulfoxide, and aldicarb sulfone residues in cotton 

undelinted seed and gin byproducts. Refer to Table B. 7 .6.2.1-2a for the 5-month study and 

Table B.7.6.2.l-2b for the 7-week study. Concurrent recoveries were used to correct the 

recoveries in the stored samples. 

The detector response was linear for aldicarb, aldicarb sulfoxide, and aldicarb sulfone 

(coefficient of determination, 1

2 0.9908) within the range of 5-1000 ng/g. Representative 

chromatograms of control samples, fortified samples, and treated samples were provided. The 

control chromatograms generally had no peaks of interest above the chromatographic 

background. The fortified sample chromatograms contained only the analyte of interest, and 

peaks were symmetrical and well defined. Apparent residues in controls were <LOQ ( <0.01 

ppm) inion both matrices. Concurrent recoveries and recoveries in stored samples were 

corrected for apparent residues in controls if present. The registrant reported recovered residues 

for the metabolites both as unconverted values and converted to parent equivalents for all storage 

intervals. Because samples were fortified separately with each analyte and because conversion 

to parent equivalents has no impact on recovery values, the recovered residues for metabolites 

reported herein do not reflect conversion to parent equivalents. 

EPA MRJD #: 48156902 

PMRA #:NA 

Pagc4ofl0 
Aldicarb [PC Code 09830 I )/Bayer CropScience 

Table B.7.6.2.l-2a. Summary of Procedural/Concurr ent Recoveries of Aldicarb, Aldicarb Sulfoxide, a nd 

Ald icarb Sulfone from Cotton Matrices: 5-Month Study. 

Matrix Analyte Fortification Storage Interval, 

Level (ppm) (Months) 

Undelinted Aldicarb 0. 10 0 

seed I 

1.3 

2 

4 

5 

Aldicarb 0.10 0 

sulfoxidc I 

1.3 

2 

4 

5 

Aldicarb 0.10 0 

sulfonc I 

1.3 

2 

4 

5 

Gin Aldicarb 0.10 0 

byproducts I 

2 

4 

5 

Aldicarb 0. 10 0 

sulfoxide I 

2 

4 

5 

/\ldicarb 0. 10 0 

sulfone I 

2 

4 

5 1 Concurrent recovenes were corrected for apparent residues in controls. 

Standard deviation is not applicable for sample sizes n<3. 

EPA MRID #: 48156902 

PMRA #: NA 

Recoveries 1 

(%) 

120, 109. 107 

98. 94 

11 0. 11 4 

87. 90 

74. 102 

79.94 

93, 8 1, 81 

84.87 

86,96 

85, 75 

90. 102 

99.96 

88, 91. 85 

94.88 

89.82 

70. 73 

103, 102 

96,93 

120, 116. 106 

99, 114 

97,93 

102.92 

98,90 

96,99.95 

87.83 

80.80 

79. 82 

83, 84 

108, 101 , 106 

92, 100 

81. 73 

96. 100 

96.92 

Mean ± Std. Dcv.2 

(%) 

112 ± 7.0 

96 

112 

89 

88 

86 

85 ± 6.9 

86 

9 1 

80 

96 

97 

88 ± 2.7 

91 

86 

72 

103 

94 

114 ± 7.2 

106 

95 

97 

94 

97± 2. 1 

85 

80 

80 

83 

105 ± 3.5 

96 

77 

98 

94 

Page5ofl0 
Aldicarb [PC Code 09830 I ]/Bayer CropScience 

Table B.7.6.2.l-2b. Summary of Procedu ral/Concurrent Recoveries of Aldica rb, Aldicarb Sulfoxide, and 

Aldicarb Sulfo ne from Cotton Undelinted Seed: 7-Wcek Study. 

Matrix Analyte Fortification Storage Interval 

Level (ppm) (Weeks) 

Undclinted seed Aldicarb 0.10 0 

I 

2 

3 

4 

7 

Aldicarb 0. 10 0 

sulfoxide I 

2 

3 

4 

7 

Aldicarb 0.10 0 

sulfone I 

2 

3 

4 

7 

1 Concurrent recoveries were corrected for apparent residues in controls. 2 Standard deviation is not applicable for sample sizes n<3. 

Recoveries1 

(%) 

104. 107. 105 

92,94 

94.86 

93.92 

73, 108 

108, 109 

IOI, IOI, 11 3 

104. 107 

108. 106 

95,90 

77, 77 

IOI , 99 

97, 102.99 

104, 11 0 

106, 117 

87. 94 

104. 11 0 

107. 112 

Mean ± Std. Dev.2 

(%) 

105 ± 1.5 

93 

90 

92 

91 

108 

105± 7.1 

106 

107 

92 

77 

100 

99 ± 2.3 

107 

111 

91 

107 

110 

The results of the storage stability study are presented in Tables B.7.6.2. l-3a (5-month study) 

and B.7.6.2. l-3b (7-week study). In the 5-month study for cotton undelinted seed, residues of 

aldicarb, aldicarb sulfoxide, and aldicarb sulfone declined following I month of frozen storage 

(recoveries of 3 1-33%), and generally appeared to stabilize at subsequent storage intervals. ln 

the 7-week study for undelinted seed, loss on storage was observed for residues of all three 

analytes at storage intervals > 15 days. When the results for both the 5-month and the 7-week 

studies are combined, the average recoveries for residues of aldicarb, aldicarb sul foxide, and 

aldicarb sulfone in/on cotton undelinted seed at all storage intervals > 15 days were 43-46% 

(overall average recovery for all three analytes of -44%). The data for cotton gin byproducts 

indicate that residues of aldicarb were stable during frozen storage for up to 4 months but 

declined by the 5-month storage interval (40% recovery), while residues of aldicarb sulfoxide 

and aldicarb sulfone were stable for at least 5 months. 

The submitted storage stability data indicate that co1Tection for loss on storage is needed for 

residues of aldicarb, aldicarb sulfoxide, and aldicarb sulfone in/on cotton undelinted seed stored 

frozen for> 15 days and for residues of aldicarb in/on samples of cotton gin byproducts stored 

frozen for >4 months. 

EPA MRJD #: 48 156902 

PMRA #:NA 

Page 6of10 
Aldicarb [PC Code 09830 I )/Bayer CropSciencc 

Table B.7.6.2.1-3a. Stability of Ald icarb, Ald icarb Sulfoxide, and Aldicarb Sulfone Residues in Cotton 

Matrices During Storage at -20 °C for up to 5 months. 

Commodity Analyte fortification 

Level (ppm) 

Undel intcd Aldicarb 0. 10 

seed 

Aldicarb 0.10 

sulfoxide 

Aldicarb 0.10 

sulfone 

Gin Aldicarb 0.10 

byproducts 

Aldicarb 0.10 

sulfoxide 

Aldicarb 0. 10 

sulfone 

. . 1 Interval from forttl1 cat1 on to cxtrac11on . 

~Corrected for concurrent recovery. 

EPAMR.ID#: 48 156902 

PMR.A #: NA 

Storage lnterval 1 

Months (Days) 

0 (0) 

I (27) 

1.3 (38) 

2 (55) 

4 (120) 

5 ( 152) 

0 (0) 

1 (27) 

1.3 (38) 

2 (SS) 

4 ( 120) 

5 ( 1 S2) 

0 (0) 

I (27) 

1.3 (38) 

2 (55) 

4 ( 120) 

5 ( 152) 

0 ( I) 

I (28) 

2 (56) 

4 ( 12 1) 

5 ( 148) 

0 ( I) 

I (28) 

2 (56) 

4 ( 121) 

5 ( 148) 

0 ( I) 

I (28) 

2 (56) 

4 ( 12 1) 

5 (148) 

Recovered Residues Mean 

(ppm) Recovery 

(%) 

0. 120, 0. 109. 0. 107 11 2 

0.0236, 0.0393 3 1 

0.0299, O.oJ 16 3 1 

0.0378, 0.0466 42 

0.0697, 0.0559 63 

0.0383, 0.0368 38 

0.0928. 0.08 12. 0.08 10 85 

0.02 17, 0.0309 26 

0.0273, 0.0300 29 

0.0232. 0.0243 24 

0.0469, 0.0346 4 1 

0.0549, 0.052S S4 

0.0881, 0.0909, 0.08SS 88 

0.027 1, 0.0330 30 

0.0209, O.D25 I 23 

0.0228, 0.0338 28 

0.0378, 0.0640 51 

0.0446. 0.0661 55 

0.12 1, 0. 11 6. 0. 106 11 4 

0.09 12, 0.0943 93 

0.0757, 0.078 1 77 

0.08 18, 0.0814 82 

0.0353. 0.0392 37 

0.0955. 0.0993. 0.0947 97 

0.0840, 0.0837 84 

0.0736. 0.078 1 76 

0.0913, 0.0791 85 

0.0782, 0.0747 76 

0. 108, 0. 102, 0.106 105 

0.0872, 0.0816 84 

0.0750, 0.0750 75 

0. 102. 0.0905 96 

0.0945, 0.0988 97 

Concurrent Corrected 

Recovery Recovcry2 

(%) (%) 

11 2 -- 96 33 

11 2 27 

89 47 

88 71 

86 44 

85 --

86 3 1 

9 1 3 1 

80 30 

96 42 

97 SS 

88 -- 9 1 33 

86 27 

72 39 

103 49 

94 59 

11 4 -- 106 88 

95 8 1 

97 84 

94 40 

97 --

85 99 

80 95 

80 107 

83 92 

105 --

96 88 

77 97 

98 98 

94 103 

Page 7of 10 
Aldicarb [PC Code 09830 I ]/Bayer CropScience 

Table B.7.6.2.l -3b.Stability of Aldica rb, Aldicarb Sulfoxide, and Aldicarb Sulfone Residues in Cotton 

Matrices During Storage at -20 °C for up to 7 weeks. 

Commodity Analyte Fortification 

Level (ppm) 

Undelinted Aldicarb 0. 10 

seed 

Aldicarb 0. 10 

sulfox ide 

Aldicarb 0. 10 

sulfone 

1 Interval from fortification to extraction. 2 Corrected for concurrent recovery. 

Storage Interval 1 Recovered Residues 

Weeks (Days) (ppm) 

0 (0) 0. 104. 0. 107, 0. 105 

1 (8) 0.0999. 0.0981 

2 ( 15) 0. 108, 0. 114 

3 (22) 0.0497. 0.0278 

4 (28) 0.0400. 0.0334 

7 (47) 0.0472. 0.0438 

0 (0) 0. 10 1, 0.1 0 1, 0. 11 4 

1 (8) 0. 101.0. 10 1 

2 ( 15) 0. 11 4. 0. 120 

3 (22) 0.0537, 0.0489 

4 (28) 0.0473. 0.0443 

7 (47) 0.05 16, 0.04 79 

0 (0) 0.0968, 0. 101. 0.0989 

I (8) 0. 100, 0. 109 

2 ( 15) 0. 109, 0. 107 

3 (22) 0.057 1, 0.0606 

4 (28) 0.0537. 0.0465 

7 (47) 0.0433, 0.06 11 

Mean Concurrent Corrected 

Recovery Recovery Rccovery2 

(%) (%) (%) 

105 105 -- 99 93 106 

111 90 123 

39 92 42 

37 9 1 40 

46 108 42 

105 105 -- 10 1 106 95 

11 7 107 109 

5 1 92 56 

46 77 59 

50 100 50 

99 99 -- 105 107 98 

108 111 97 

59 9 1 65 

50 107 47 

52 11 0 47 

Graphs of the storage stability of residues of aldicarb, aldicarb sulfoxide, and aldicarb sulfone 

during frozen storage inion cotton undelinted seed and gin byproducts are presented in Figures 

B.7.6.2.1-l (cotton undelinted seed, 5-month study), B.7.6.2.1-2 (cotton undelinted seed, 7-week 

study), and 8.7.6.2. 1-3 (cotton gin byproducts). 

EPA MRJD #: 481 56902 

PMRA #: NA 

Page 8of10 
Aldicarb [PC Code 09830 I ]/Bayer CropScience 

Figure B.7.6.2.1-1 Graph of Aldicarb and Metabolites in Cotton Undelinted Seed Stored for 

up to S Months 

120 

* 100 > 

Qj 

> 80 0 

u 

Cl) 

0: 60 -0 

Cl) 

..., 

u 40 Cl) 

'-

0 20 u 

0 

Storage Stability of Aldicarb and Metabolites in Cotton 

Undelinted Seed 

0 20 40 60 80 100 120 140 

Storage Interval (Days) 

_._.. Ald1carb - - Ald1carb sulfoxide _._.. Ald1carb Sulfone 

160 

Figure B.7.6.2. 1-2 Graph of Aldicarb and Metabolites in Cotton Undelinted Seed Stored for 

up to 7 Weeks 

140 

* 120 

2:"' 

Cl) 100 > 

0 

u 80 Cl) 

0: 

-0 60 Cl) 

u 40 ~ 0 

u 20 

0 

Storage Stability of Aldicarb and Metabolites in Cotton 

Undelinted Seed 

0 10 20 30 40 

Storage Interval (Days) 

_._Aldicarb --<i Aldicarb sulfox1de -.-Aldicarb Sulfone 

EPA MRID #: 48 156902 

PMRA #: NA 

50 

Page 9of10 
Aldicarb [PC Code 09830 I )/Bayer CropScicnce 

Figure B.7.6.2.1-3 Graph of Aldicarb and Metabolites in Cotton Gin Byproducts Stored for 

up to 5 Months 

120 

'*-

> 

(jj 

> 80 0 

u 

Q) 

a:: 60 "O 

~ u 40 ~ .... 

0 

u 20 

0 

Storage Stability of Aldicarb and Metabolites in Cotton 

Gin Byproducts 

0 20 40 60 80 100 120 140 

Storage Interval (Days) 

-+-Aldicarb -+-Aldicarb sulfoxide ...,._ Aldicarb Sulfone 

III. CONCLUSIONS 

160 

The storage stability study with cotton is considered scientifically acceptable. In the 5-month 

study for cotton undelinted seed, residues of aldicarb, aldicarb sulfoxide, and aldicarb sulfone 

declined following l month of frozen storage (recoveries of 31-33%), and generally appeared to 

stabilize at subsequent storage intervals. In the 7-week study for undelinted seed, loss on storage 

was observed for residues of all three analytes at storage intervals > 15 days. When the results 

for both the 5-month and the 7-week studies are combined, the average recoveries for residues of 

aldicarb, aldicarb sulfoxide, and aldicarb sulfone in/on cotton undelinted seed at all storage 

interva ls> 15 days were 43-46% (overall average recovery for all three analytes of - 44%). The 

data for cotton gin byproducts indicate that residues of aldicarb were stable during frozen storage 

for up to 4 months but declined by the 5-month storage interval (40% recovery), while residues 

of aldicarb sulfoxide and aldicarb sulfone were stable for at least 5 months. 

The submitted storage stability data indicate that correction for loss on storage is needed for 

residues of aldicarb, aldicarb sulfoxide, and aldicarb sulfone in/on cotton undelinted seed stored 

frozen for > 15 days and for residues of aldicarb in/on san1ples of cotton gin byproducts stored 

frozen for >4 months. 

REFERENCES 

None. 

EPA MR1D #: 48156902 

PMRA #: NA 

Page 10of10 
Volume 3 

Annex B 

Aldicarb 

B.5 METHODS OF ANALYSIS 

B.5.2 ANALYTICAL METHODS FOR THE DETERMINATION OF RESIDUES 

(ALL COMPONENTS INCLUDED IN THE RESIDUE DEFINITION PROPOSED) 
Aldicarb [PC Code 09830 I)/ Bayer CropScience 

Table B.5.2-1. Overview of the Ana lytical Methods for the Determina tion of Aldicarb Residues. 

Data Matrix Analytes Method Type Limit of Reference 

Requirement Quantitation (ppm) 

Enforcement Not speci lied Total aldicarb GLC/FPD 0.01-0.05 PAM Vol. II. Methods I 

Methods - Plant residues detem1ined (Method 11) (LOO) and II and Methods /I. 

Commodities as aldicarb sulfone and B. Residue 

Cottonseed Not specified GLC/FPD 0.02 Chemistry Chapter for 

(Method I similar to (LOO) Aldicarb RED. 

Method II) DP#266396. C. Swartz. 

Cottonseed Not specified Colorimetric 0.03 6/2/00 

(Method A) (LOO) 

Oranges Not specified GC/FPD ot specified 

(Method B. similar to 

Method II except 

nonpolar GC column 

used) 

Data-Gathering Potato Aldicarb LC/MS/MS 0.01 Study No. MR-085/04 

Method- Plant Orange peel Aldicarb sulfoxide MRID 48156903 

Commodities Orange pulp Aldicarb sulfone 

Potato tubers Aldicarb HPLC 0.02. for each Residue Chemistry 

Aldicarb sulfoxide (Method RPAC SOP analyte Chapter for Aldicarb 

Aldicarb sulfone 90015) (LOD = 0.0 I ppm) R.EO, DP#266396. C. 

Swartz, 6/2/00 

Enforcement Milk Not specified GLC/FPD 0.00 1 PAM Vol. II. Method 

Method- (Method Ill similar to (LOO) Ill, Residue Chemistry 

Livestock Method II) Chapter for Aldicarb 

Commodities RED. DP#266396. C. 

Swartz. 6/2/00 

Multiresidue FDA-Pesticide Residue Chemistry 

Method Testing Analytical Methods Chapter for Aldicarb 

Multi-Residue testing RED. DP#266396. C. 

program Swartz. 6/2/00 

Table B.5.2-2. C hemical Structures of Ana lytes Addressed by Methods for the Analysis of Aldicarb. 

Method ID Chemical Name 

0085 1 Aldicarb 

Aldicarb sulfoxidc 

EPA MRJD #: 48 156903 

PMRA #: NA 

Chemical Structure 

CH3 0 

I 11 ,.H 

CHrS·C-CH = N-0-C-N 

I ' CH3 CH3 

0 CH3 0 

II I II 

CH3S-C-CH=N-OCNHCH;s 

I 

CH 3 

Page2of6 
Aldicarb [PC Code 09830 I)/ Bayer CropScience 

Table B.S.2-2. Chemical Structures of Analytes Addressed by Methods for the Analysis of Aldicarb. 

Method ID Chemical Name Chemica l Structure 

Aldicarb sulfone H3C\ /'° N-C CH3 

/ \ I 

H O- N=CH- C- CH3 I 

O=S=O 

I 

CH3 

Note: This Data Evaluation Record (DER) was originally prepared under contract by Versar, Inc. (6850 Versar Center, 

Springfield. VA 22 15 1; submitlcd 3/ 13/15). The DER has been reviewed by I IED and revised to re flect current Office of 

Pesticide Programs (OPP) po licies. 

B.5.2.1 Analytical Methods for Plant Matrices (Annex IIA 4.3, Annex IIIA 5.3) 

B.5.2.l .1 Post-Registration Method (Enforcement) 

Not Applicable 

B.5.2.1.2 Pre-Registration Method (Data-Gathering) 

Document ID: MRID No. 48156903 

Report: Analytical Method 00851 for the Determination of Residues of Aldicarb 

and Its Metabolites Aldicarb Sulfone and Aldicarb Sulfoxide in Potatoes 

and Oranges by LCMSMS. Report Number: MR-085/04. Unpublished 

study prepared by Bayer CropScience. 57 p. 

Guidelines: EPA OCSPP Harmonized Test Guideline 860.1340 Residue Analytical 

Method (August 1996) 

PMRA Regulatory Directive DIR98-02 - Residue Chemistry Guidelines, 

Section 3 - Residue Analytical Method 

EU SANCO 825/00/rev. 7 (17/3/04) 

OECD Guidance Document on Pesticide Residue Analytical Methods 

GLP Compliance: No deviations from regulatory requirements were reported which would 

have an impact on the validity of the study. 

Acceptability: The study is considered scientifically acceptable. The acceptability of this 

study for regulatory purposes is addressed in the forthcoming U.S. EPA 

Residue Chemistry Summary Document, DP# 425180. 

Evaluator: William H. Donovan, Ph.D., Chemist, RABY 

EXECUTIVE SUMMARY 

Bayer CropScience has submitted a high perfonnance liquid chromatography method with 

tandem mass spectrometry detection (LC/MS/MS), Method 0085 1, for the determination of 

residues of aldicarb and its metabolites aldicarb sulfone and aldicarb sulfoxide in potatoes and 

oranges. The method was used for analysis of aldicarb and its metabolites aldicarb sulfone and 

aldicarb sulfox ide in the cotton magnitude of the residue crop field trials and freezer storage 

stability studies. A complete method description and validation data were submitted. 

EPA MRID #: 48 156903 

PMRA #:NA Page 3 of6 
Aldicarb [PC Code 09830 I)/ Bayer CropScience 

Briefly, samples were extracted twice with dichloromethane (DCM):acetone (75 :25, v:v) and 

filtered. The extracts were combined and diluted with DCM/acetone. Ethylene glycol was 

added, and the mixture was concentrated, reconstituted in acetonitrile and diluted buffer 

(ammonium acetate and acetic acid diluted with water), and filtered. The filtrate was diluted 10 

times using either the diluted buffer or the dilution mixture containing reserpine as injection 

standard for LC/MS/MS analysis. The method monitors a single ion transition for aldicarb (208 

mlz--+ 11 6 m/z), aldicarb sulfone (223 m/z--+ 76 m/z), aldicarb sulfox ide (207 m/z --+ 132 m/z), 

and reserpine (609.3 mlz--+ 195. l m/z) [internal standard]. The limit of quantitation (LOQ; 

determined as the lowest level of method validation, LLMY) is 0.0 1 ppm for each analyte. 

The method was adequately validated using samples of potato, orange pul p, and orange peel 

fortified with each analyte at 0.0 1 and 0.1 0 ppm. Recoveries were generall y within the 

acceptable range of 70-1 20% for all matrices and analytes. 

IL V data were not submitted to the Agency; however, because IL V is not generally required for 

data collection methods, no additional information is required. 

l. Principle of the Method: Method 00851 

Table B.5.2. 1.2-1. Summary Parameters for the Pre-Registration Analytical Method Used for the Analysis 

of Aldicarb Residues in Potato, Orange Peel, and Orange Pulp. 

Method ID 

Analytc(s) 

Extraction solvent and 

technique 

Clean-up strategics 

Instrument and Detector 

Standardization method 

Stability of std solutions 

Retention times 

EPA MRID #: 48156903 

PMRA #: NA 

0085 1 

/\ldicarb. Aldicarb sulfoxide, and Aldicarb sulfonc 

Samples were extracted twice with dichloromethane (OCM):acetonc (75:25. v:v) and filtered. 

Tite extracts were combined and diluted with DCM/acetone. Ethylene glycol was added. and the 

mixture was concentrated, reconstituted in acetonitrile and diluted bufTcr (ammonium acetate and 

acetic acid diluted with water). and filtered. The filtrate was diluted 10 times using either the 

diluted bufTer or the dilution mixture (diluted bufTer with I ug/L reserpine) for analysis. 

None 

I I PLC/MS/MS using a Phenomcnex AQUA C 18 column (and gradient mobi le phase of water 

with 1.5% acetic acid and ammonium acetate JO mM, and acctonitri lc. MS/MS detection 

operated in positive ionization mode under multiple reaction monitoring (MRM) conditions. 

The fo llowing ion transitions arc monitored: 

/\ldicarb: ml= 208-+ 11 6 

/\ldicarb sulfoxidc: 111/::: 207-+ 132 

/\ldicarb sulfone: ml= 223-+76 

Reserpine: 111/: 609.3-- 195. I 

External standardization using a 6-point calibration curve to generate a standard curve through 

linear regression analysis. 

Standard stock solutions (I 000 ~1g/ml). fortification standards (I 0 and 1.0 μg/ml). and calibration 

solutions of aldicarb. in acetonitrile were reported to be stable for 2 months when stored at 5 ± 3 

°C. /\ldicarb sulfoxide and alclicarb sulfonc stock solutions were reported to be stable for 6 

months when stored at 5 ± 3 °C. 

f-i nal extracts stored at I 0 °C were found to be stable for up to 7 days for potato. 3 days for 

orange pulp. and 4 days for orange peel. 

Aldicarb - 5.9 minutes 

Aldicarb sulfoxidc - 2.8 minutes 

/\ldicarb sulfone -4.0 minutes 

Reserpine -5.9 minutes 

Page 4 of6 
A ldicarb [PC Code 09830 I)/ Bayer CropScience 

II. Specificity 

The LC/MS/MS method is highly selective for the quantitation of aldicarb and its metabolites 

aldicarb sulfoxide and aldicarb sulfone. Analysis of control samples resulted in no significant 

signals at the expected retention times of the analytes. The petitioner indicated that there was no 

interference with other substances observed at the retention times of aldicarb and its metabolites 

aldicarb sulfoxide and aldicarb sulfone above 30% of the LOQ. The following ion transitions are 

monitored: 

Aldicarb 

Alidcarb sulfoxide 

Aldicarb sulfone 

Reserpine 

III. Linearity 

nzlz 208-116 (quantitation) 

mlz 207-132 (quantitation) 

mlz 223-76 (quantitation) 

m/z 609.3-195. l (quantitation) [internal standard] 

For each analyte, the linearity of detector response was evaluated using solvent standard 

solutions. Calibration curves were calculated by linear regression analysis with l/x weighting. 

For the least-squares equation, which describes the detector response as a function of the 

standard concentration, calibration curves resulting from the injection of a minimum of 6 

standards over the concentration range of 0.04-5 μg/L demonstrated linearity with coefficients of 

determination (r2) of at least 0.9990. 

IV. Accuracy (Recovery) and Precision (Repeatability) 

No radiovalidation data were included in the submission. Analytical methods should be 

radiovalidated to determine whether total toxic residues (TTR) are extracted from weathered 

matrices. 

The method was adequately validated for the quantitation ion transition using samples of potato, 

orange peel, and orange pulp fortified with either a mixed standard or each analyte separately at 

0.0 I and 0.10 ppm. Recoveries were generally within the acceptable range of 70-120%. The 

individual recoveries were within the range of 67-117%. While there were two recoveries from 

a total of I 08 measurements that were 67%, the mean recoveries were at least 70% with relative 

standard deviations S20%. At the 0.01 ppm level (LOQ), the mean recoveries were within the 

range of78-1 00%, with relative standard deviations within the range of2.3- l5%. At the 0.10 

ppm level (1 Ox LOQ), the mean recoveries were within the range of 83-102%, with relative 

standard devi ations within the range of 1.6-7 .5%. 

Repeatability data were generated from at least 18 samples fortified at the LOQ and at least 18 

samples fortified at I Ox LOQ for each matrix and analyte. The standard deviations (RSDs) 

obtained for each fortification level were less than 20%. Recovery and repeatability data are 

presented in Table B.5.2.1 .2-2, below. 

Table B.5.2.1.2-2. Accuracy and Precision Data for Method 00851. 

Analytc Matrix 

Aldicarb Potato 

EPA MRID #: 48156903 

PMRA #: NA 

Fortification 

Level (ppm) 

0.010 

Concurrent Recovery(%) 

lndividual 1 Mean 

67,88,83.86, 89,84 83 

RSD 

Range (%) 

67-89 9.8 

Page 5 of6 
Aldicarb [PC Code 09830 I)/ Bayer CropScience 

Ta ble B.5.2.1.2-2. Accur acy a nd Precision Da ta for Method 0085 1. 

Analyte Matrix Fortification Concurrent Recovery (%) RSD 

Level (ppm) Individual' Mean Range (%) 

0.100 81. 84, 77.82. 95, 80 83 77-95 7.5 

Orange peel 0.010 89, 99, 99, 103. 99. 98 98 89-103 4.8 

0.100 92.94.90,89.93. 102 93 89-102 5.0 

Orange pulp 0.010 91. 73. 83, 9 1. 83, 82 84 73-9 1 8.0 

0.100 90, 91 , 91. 87, 92, 93 91 87-93 2.3 

Aldicarb Potato 0.010 117. 83. 83, 84, 86, 90 91 83-117 14.6 sulfoxide 

0.100 104, 102, 91, 97, 96, 85 96 85-104 7.3 

Orange peel 0.010 88.83. 84.87.87, 86 86 83-88 2.3 

0. 100 102, 102. 99, 100, 104, 97 10 1 97-104 2.5 

Orange pulp 0.010 89.67. 74, 80. 78.81 78 67-89 9.4 

0. 100 84,84. 86,85, 90. 90 87 84-90 3.2 

Aldicarb sulfone Potato 0.010 95.83,83.86, 80. 74 84 74-95 8.3 

0.100 96, 96. 98. 99, 98, 100 98 96-100 1.6 

Orange peel 0.010 95. 104. 100. 104. 98, 98 100 95-104 3.6 

0.100 103. 106. 100, 98. 102, 105 102 98-106 2.9 

Orange pulp 0.010 92. 75. 95.94. 92. 93 90 75-95 8.3 

0. 100 94.99. 94,91 , 97,95 95 9 1-99 2.9 

'The first five recovery results were fortified with a mixed standard and the last result (boldcd) was fortified with each compound 

separately. 

V. Limit of Quantitation 

Table B.5.2.1.2-3. Summary of Detection a nd Quantitation Limits for Method 0085 1. 

Analyte Matrix LOD (ppm)' LOQ (ppmf 

Aldicarb Potato Not reported 0.01 

Orange peel 

Orange pulp 

Aldiearb sulfoxide Potato Not reported 0.01 

Orange peel 

Orange pulp 

/\ldicarb sulfone Potato Not reported 0.01 

Orange peel 

Orange pulp 1 LOO = limit of detection, no value reported. 2 LOO = limit of quantitation, determined as the lowest level of method validation (LLMV). 

VI. Conclusions 

The LC/MS/MS Method, 00851 , was adequately validated for determining residues of aldicarb 

and its metabolites aldicarb sulfoxide and aldicarb sulfone in potato, orange peel, and orange 

pulp. The validated LOQ is 0.0 I ppm. The analytical procedure used in the storage stability and 

crop field trial studies (MRlDs 48156902 and 48 156901 , respectively) has been successfully 

validated for aldicarb in terms of specificity, linearity, precision, accuracy, and LOQ. 

EPA MRID #: 48156903 

PMRA #:NA Page 6 of6