OFFICE OF CHEMICAL SAFETY 

AND POLLUTION PREVENTION 

UNITED STATES ENVIRONMENTAL PROTECTION AGENCY

WASHINGTON, D.C. 20460 

January 20, 2015 

 PC Code: 098301 

MEMORANDUM DP Barcode: 424560 

SUBJECT: Transmittal of a Data Evaluation Record for Analytical Methods for Aldicarb and 

Two Degradates 

FROM: Edmund Wong, Environmental Chemist 

 Greg Orrick, Environmental Scientist (Reviewer) 

Environmental Risk Branch 2 

Environmental Fate and Effects Division (7507P) 

THRU: Brian Anderson, Branch Chief 

 Environmental Risk Branch 2 

Environmental Fate and Effects Division (7507P) 

TO: Susan Bartow, Chemical Risk Manager 

 Kevin Costello, Acting Branch Chief 

 Risk Management and Implementation Branch IV 

 Pesticide Re-evaluation Division (7508P) 

 This memorandum is to inform you that the analytical method for aldicarb, aldicarb 

sulfone, and aldicarb sulfoxide in water (ECM & ILV) have been reviewed and finalized. Study 

MRIDs and classification are listed in Table 1 below.

Table 1. DER for Environmental Fate Studies of Aldicarb & Degradates 

MRID Study Type 

(OCSPP Guideline) DER Electronic File Name(s) Study 

Classification

49515901 

&

49515902 

Environmental Chemistry 

Method in Water & 

Independent Laboratory 

Validation 

(850.6100) 

098301_49515901_49515902_DER-Fate_850.6100_1-15-

15.docx Acceptable 

Anderson, Brian 

2015.01.26 

11:20:30 -05'00'

2015.01.26 

14:26:17 -05'00'
Aldicarb (PC 098301) MRID 49515901, 49515902

Analytical method for aldicarb, aldicarb sulfone, and aldicarb sulfoxide in water

Reports: ECM: MRID 49515901. Bianca, C. 2014. Method Validation of Aldicarb, 

Aldicarb Sulfone, and Aldicarb Sulfoxide in Three Water Types: Surface 

Water; Ground Water; and Drinking Water: Final Report. Project Number: 

AU/2014/03. Unpublished study prepared by JRF America. 193p.

ILV: MRID 49515902. Rutt, D.; Budgeon, A. 2014. Independent Laboratory 

Validation of JRF America Analytical Method AU-269R0 “Analytical 

Method for Analysis of Aldicarb, Aldicarb Sulfone, and Aldicarb Sulfoxide 

in Three Water Types: Surface Water, Ground Water, and Drinking Water: 

Final Report. Project Number: AU/2014/09. Unpublished study prepared by 

JRF America. 169p.

Document No.: MRIDs 49515901 & 49515902

Guideline: 850.6100

Statements: The method validations were conducted in compliance with FIFRA GLP or 

UK GLP standards. Signed and dated No Data Confidentiality Claims, GLP 

Compliance, Quality Assurance, Certification of Authenticity, and Report 

Approval statements were provided for the ECM and ILV reports.

Classification: This analytical method is classified as acceptable. It was independently 

validated upon the first attempt.

PC Code: 098301

Primary 

Reviewer: Edmund Wong Signature:

Environmental Chemist Date: Jan. 13 2015

Secondary 

Reviewer:

Gregory Orrick Signature:

Environmental Scientist Date: Jan. 13, 2015

Executive Summary

This analytical method, AU-269R0, is designed for the quantitative determination of aldicarb, 

aldicarb sulfone, and aldicarb sulfoxide in three water types: surface water, ground water, and 

drinking water using LC-MS/MS (see Table 1). The method is quantitative for the analytes at the 

stated LOQ of 0.1 μg/L. The ILV was performed in the same laboratory facility that the method 

was developed; however, the study director, analysts, instruments, and chemicals were distinct 

from those of the initial validation. The independent laboratory was successful at validating the 

method. Although several ECM LOD and LOQ recoveries for Aldicarb Sulfone and Aldicarb 

Sulfoxide were either at baseline noise level or 2x the value, all mean recoveries were within the 

acceptable range of 70-110% and RSD ≤20% for LOQ and 10xLOQ in the primary and 

confirmatory analyses. The method is repeatable and reproducible. 

Table 1. Analytical Method Summary

Analyte(s) by 

Pesticide

MRID

EPA 

ReviewMatrix Method Date Registrant Analysis

Limit of 

Quantitation

(LOQ)

Environmental 

Chemistry 

Method

Independent 

Laboratory 

Validation

Aldicarb, Aldicarb 

Sulfone, & Aldicarb 

Sulfoxide

49515901 49515902 - Water 10/15/14 AgLogic 

LLC

LCMS/MS 0.1 μg/L

1
Aldicarb (PC 098301) MRID 49515901, 49515902

I. Principle of the Method

Fortified surface, ground or drinking water samples (10 mL) were vortexed, centrifuged and then 

analysed by LC-MS/MS in positive ion mode. The method quantifies residues of aldicarb, 

aldicarb sulfone, and aldicarb sulfoxide in water at the stated LOQ of 0.1 μg/L, 10xLOQ of 1.0 

μg/L, and LOD of 0.05 μg/L. Each analyte were determined in surface, ground, and drinking 

water with primary and confirmatory analyses. 

The ILV was performed in the same laboratory facility that the method was developed. To 

ensure impartiality and independence, the study director, analysts, instruments, chemicals, 

analytical standards, etc. were “distinct and operated separately and without collusion for the 

validation portion.” The study director and analysts had no prior experience using the method. 

One attempt per matrix was performed during the course of the ILV.

II. Recovery Findings

Initial Validation Method Recoveries for Analytes in Surface, Ground, and Drinking

Water

Primary analysis mean recoveries and relative standard deviations (RSD) were within guideline 

requirements (aldicarb mean 102-105%, RSD ≤20%; aldicarb sulfone mean 101-109%, RSD 

≤20%; aldicarb sulfoxide mean 103-107%, RSD ≤20%) for LOQ and 10xLOQ samples. 

Meanwhile, confirmatory mean recoveries of LOQ and 10xLOQ were 102-105% for aldicarb, 

97-107% for aldicarb sulfone, and 102-106% for aldicarb sulfoxide. RSD of all analytes in 

confirmatory analysis were ≤20%.

Table 2. Initial Validation Method Recoveries for Analytes in Surface Water

Analyte Fortification

Level (units)

Number 

of Tests

Recovery 

Range (%)

Mean 

Recovery (%)

Standard 

Deviation (%)

Relative Standard 

Deviation (%)

Aldicarb

Primary Transition (m/z 208 → 88.6)

0.1 μg/L 7 93.4-110 102 5.9 5.7

1 μg/L 5 101-108 104 2.6 2.5

Confirmatory Transition (m/z 208 → 115.7)

0.1 μg/L 7 94-110 102 7.1 7.0

1 μg/L 5 101-107 102.6 2.5 2.4

Aldicarb Sulfone

Primary Transition (m/z 240 → 75.5)

0.1 μg/L 7 81.5-115 103 11.3 11

1 μg/L 5 104-118 108.8 5.4 5.0

Confirmatory Transition (m/z 240 → 86)

0.1 μg/L 7 89.6-116 105 9.0 8.6

1 μg/L 5 104-109 106.6 1.8 1.7

Aldicarb Sulfoxide

Primary Transition (m/z 207 → 88.5)

0.1 μg/L 7 91.7-117 104 9.2 8.9

1 μg/L 5 105-110 107 2.0 1.9

Confirmatory Transition (m/z 207 → 68.5)

0.1 μg/L 7 85-117 102 10.7 10.5

1 μg/L 5 104-110 106.2 2.3 2.1

2
Aldicarb (PC 098301) MRID 49515901, 49515902

Table 3. Initial Validation Method Recoveries for Analytes in Ground Water

Analyte Fortification

Level (units)

Number 

of Tests

Recovery 

Range (%)

Mean 

Recovery (%)

Standard 

Deviation (%)

Relative Standard 

Deviation (%)

Aldicarb

Primary Transition (m/z 208 → 88.6)

0.1 μg/L 7 102-109 105 2.5 2.4

1 μg/L 5 103-105 104 0.8 0.8

Confirmatory Transition (m/z 208 → 115.7)

0.1 μg/L 7 101-110 104 3.2 3.1

1 μg/L 5 101-105 103 1.5 1.4

Aldicarb Sulfone

Primary Transition (m/z 240 → 75.5)

0.1 μg/L 7 101-112 107 3.4 3.2

1 μg/L 5 104-110 107 2.6 2.4

Confirmatory Transition (m/z 240 → 86)

0.1 μg/L 7 87.9-107 98 7.9 8.0

1 μg/L 5 105-108 106 1.1 1.1

Aldicarb Sulfoxide

Primary Transition (m/z 207 → 88.5)

0.1 μg/L 7 101-110 105 3.3 3.2

1 μg/L 5 101-106 103 2.3 2.2

Confirmatory Transition (m/z 207 → 68.5)

0.1 μg/L 7 90.4-109 102 7.0 6.9

1 μg/L 5 100-109 104 3.7 3.6

Table 4. Initial Validation Method Recoveries for Analytes in Drinking Water

Analyte Fortification

Level (units)

Number 

of Tests

Recovery 

Range (%)

Mean 

Recovery (%)

Standard 

Deviation (%)

Relative Standard 

Deviation (%)

Aldicarb

Primary Transition (m/z 208 → 88.6)

0.1 μg/L 7 101-108 104 2.6 2.5

1 μg/L 5 101-109 105 2.9 2.8

Confirmatory Transition (m/z 208 → 115.7)

0.1 μg/L 7 102-109 105 2.4 2.2

1 μg/L 5 100-106 103 2.6 2.5

Aldicarb Sulfone

Primary Transition (m/z 240 → 75.5)

0.1 μg/L 7 93-112 101 6.0 6.0

1 μg/L 5 98.6-108 102 3.5 3.4

Confirmatory Transition (m/z 240 → 86)

0.1 μg/L 7 85.3-108 97 7.9 8.2

1 μg/L 5 102-109 106 2.9 2.7

Aldicarb Sulfoxide

Primary Transition (m/z 207 → 88.5)

0.1 μg/L 7 97.8-112 106 4.4 4.2

1 μg/L 5 101-107 104 2.3 2.2

Confirmatory Transition (m/z 207 → 68.5)

0.1 μg/L 7 97.8-113 106 5.4 5.1

1 μg/L 5 102-110 106 3.3 3.1

3
Aldicarb (PC 098301) MRID 49515901, 49515902

Independent Validation Method Recoveries for Analytes in Surface, Ground, and Drinking

Water

Primary analysis mean recoveries and relative standard deviations (RSD) were within guideline 

requirements (aldicarb mean 100-106%, RSD ≤20%; aldicarb sulfone mean 93.4-106%, RSD 

≤20%; aldicarb sulfoxide mean 93.5-106%, RSD ≤20%) for LOQ and 10xLOQ samples. 

Meanwhile, confirmatory mean recoveries of LOQ and 10xLOQ were 100-106% for aldicarb, 

89.4-107% for aldicarb sulfone, and 91-101% for aldicarb sulfoxide. RSD of all analytes in 

confirmatory analysis were ≤20%.

Table 5. Independent Validation Method Recoveries for Analytes in Surface Water

Analyte Fortification

Level (units)

Number 

of Tests

Recovery 

Range (%)

Mean 

Recovery (%)

Standard 

Deviation (%)

Relative Standard 

Deviation (%)

Aldicarb

Primary Transition (m/z 208 → 88.6)

0.1 μg/L 5 85.2-110 101 10.5 10.3

1 μg/L 5 92.6-107 102 5.8 5.7

Confirmatory Transition (m/z 208 → 115.7)

0.1 μg/L 5 78.4-110 100 12.5 12.5

1 μg/L 5 86.8-113 103 10.2 9.9

Aldicarb Sulfone

Primary Transition (m/z 240 → 75.5)

0.1 μg/L 5 72.5-104 93.4 12.5 13.4

1 μg/L 5 89.7-103 95.9 5.0 5.2

Confirmatory Transition (m/z 240 → 86)

0.1 μg/L 5 82.6-95.9 89.4 5.3 5.9

1 μg/L 5 88.2-104 93.7 6.2 6.7

Aldicarb Sulfoxide

Primary Transition (m/z 207 → 88.5)

0.1 μg/L 5 92.8-103 96.7 4.1 4.2

1 μg/L 5 86.2-97.9 93.5 4.5 4.9

Confirmatory Transition (m/z 207 → 68.5)

0.1 μg/L 5 88.6-101 96.9 5.5 5.7

1 μg/L 5 87.1-109 101 8.6 8.5

Table 6. Independent Validation Method Recoveries for Analytes in Ground Water

Analyte Fortification

Level (units)

Number 

of Tests

Recovery 

Range (%)

Mean 

Recovery (%)

Standard 

Deviation (%)

Relative Standard 

Deviation (%)

Aldicarb

Primary Transition (m/z 208 → 88.6)

0.1 μg/L 5 89.1-110 101 8.0 7.9

1 μg/L 5 89.7-112 100 8.9 8.9

Confirmatory Transition (m/z 208 → 115.7)

0.1 μg/L 5 97.7-110 103 6.2 6.0

1 μg/L 5 96.1-113 106 6.3 5.9

Aldicarb Sulfone

Primary Transition (m/z 240 → 75.5)

0.1 μg/L 5 99.4-110 105 4.3 4.1

1 μg/L 5 89-104 98.1 6.2 6.3

Confirmatory Transition (m/z 240 → 86)

0.1 μg/L 5 103-110 107 3.1 2.9

1 μg/L 5 98.4-109 105 3.9 3.7

4
Aldicarb (PC 098301) MRID 49515901, 49515902

Aldicarb Sulfoxide

Primary Transition (m/z 207 → 88.5)

0.1 μg/L 5 93.9-107 98.3 5.2 5.3

1 μg/L 5 93.2-109 100 5.8 5.8

Confirmatory Transition (m/z 207 → 68.5)

0.1 μg/L 5 72.9-107 92.6 13.4 14.5

1 μg/L 5 77.3-110 91.9 12.2 13.3

Table 7. Independent Validation Method Recoveries for Analytes in Drinking Water

Analyte Fortification

Level (units)

Number 

of Tests

Recovery 

Range (%)

Mean 

Recovery (%)

Standard 

Deviation (%)

Relative Standard 

Deviation (%)

Aldicarb

Primary Transition (m/z 208 → 88.6)

0.1 μg/L 5 98-110 106 5.2 4.9

1 μg/L 5 90.7-110 102 7.6 7.4

Confirmatory Transition (m/z 208 → 115.7)

0.1 μg/L 5 92.6-110 106 8.4 8.0

1 μg/L 5 9.31-107 100 5.8 5.8

Aldicarb Sulfone

Primary Transition (m/z 240 → 75.5)

0.1 μg/L 5 100-109 106 6.7 6.3

1 μg/L 5 95.4-110 103 6.9 6.7

Confirmatory Transition (m/z 240 → 86)

0.1 μg/L 5 97.6-108 104 3.9 3.8

1 μg/L 5 99.4-110 100 6.7 6.7

Aldicarb Sulfoxide

Primary Transition (m/z 207 → 88.5)

0.1 μg/L 5 95.1-111 106 6.7 6.3

1 μg/L 5 96.2-103 102 5.0 4.9

Confirmatory Transition (m/z 207 → 68.5)

0.1 μg/L 5 83-103 91 7.5 8.2

1 μg/L 5 88.2-113 98.9 11.1 11.2

III.Method Characteristics

5
Aldicarb (PC 098301) MRID 49515901, 49515902

The LOD was considered to be a concentration equivalent to 50% of the stated LOQ (0.1 μg/L), 

which is 0.05 μg/L for aldicarb, aldicarb sulfone, and aldicarb sulfoxide. In some cases, the 

LOD was lowered to 24% of the LOQ (0.024 μg/L) dependent upon the sensitivity, linear range, 

and conditions of the LC/MS/MS system. The stated LOQ was determined as the lowest 

fortification concentration with adequate accuracy (mean recoveries within 70-120%) and 

precision (RSDs ≤20%). 

The LOD and LOQ values were >10x the baseline noise in the control samples for aldicarb in 

surface, ground, and drinking water. However, the LOD was <1x the baseline noise in drinking 

water samples for aldicarb sulfone. The LOQ was about 2x baseline noise for surface, ground 

and drinking water for aldicarb sulfone. For aldicarb sulfoxide, the LOD was 2x the baseline 

noise in drinking water samples, while the LOQ was >4x baseline noise for surface, ground, and 

drinking water.

The method was reproducible for all analytes in surface, ground, and drinking water at the stated 

LOQ of 0.1 μg/L.

Table 4. Method Characteristics

Aldicarb Aldicarb Sulfone Aldicarb Sulfoxide

Limit of Quantitation (LOQ) 0.1 μg/L 0.1 μg/L 0.1 μg/L

Limit of Detection (LOD) 0.05 μg/L 0.05 μg/L 0.05 μg/L

Linearity (calibration curve r2

and concentration range)

r

2 = 0.995

(0.05 – 1.0 μg/L)

r

2 = 0.995

(0.05 – 1.0 μg/L)

r

2 = 0.995

(0.05 – 1.0 μg/L)

Repeatable Yes (RSD <20%) Yes (RSD <20%) Yes (RSD <20%)

Reproducible Yes Yes Yes

Specific Yes Yes Yes

IV.Method Deficiencies and Reviewer’s Comments

In the ECM, for aldicarb sulfone, the LOD was at the baseline noise level in drinking water 

samples, while the LOQ was about 2x baseline noise for surface, ground and drinking water. For 

aldicarb sulfoxide, the LOD was calculated as 2x the baseline noise in drinking water samples. 

However, mean recoveries for all analytes (aldicarb, aldicarb sulfone, and aldicarb sulfoxide) 

were within the acceptable range of 70-120% and RSD ≤20% in surface, ground, and drinking 

water.

No other major deficiencies with the method were found.

6
Aldicarb (PC 098301) MRID 49515901, 49515902

Attachment 1: Chemical Names and Structures

Table 1. Aldicarb, Aldicarb Sulfone, and Aldicarb Sulfoxide. A

Code Name/ Synonym Chemical Name Chemical Structure

Aldicarb IUPAC: 2-methyl-2(methylthio)propionaldehyde O-(methylcarbamoyl)oxime

CAS No.: 116-06-3

Formula: C7H14N2O2S

MW: 190.26 g/mol

SMILES: C(C)(C)(C=NOC(=O)NC)SC

Aldicarb Sulfone IUPAC: [(E)-(2-methyl-2-methylsulfonylpropylidene)amino] N-methylcarbamate

CAS No.: 1646-88-4

Formula: C7H14N2O4S

MW: 222.26 g/mol

SMILES: CC(C)(/C=N/OC(=O)NC)S(=O)(=O)C

Aldicarb Sulfoxide IUPAC: (E)-(2-methanesulfinyl-2-methylpropylidene)amino N-methylcarbamate

CAS No.: 1646-87-3

Formula: C7H14N2O3S

MW: 206.263 g/mol

SMILES: CNC(=O)O\N=C\C(C)(C)S(C)=O

A MW means “molecular weight”. 

C

CH3

S

CH3

CH3

O N

O

N

H

H3C

H

7