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iMethod Test for Cliquid Software

Experimental Conditions to Analyze Carbamate Pesticides

Important InformationIntroductionInstrumentationChemicalsSample Preparation Procedures

Preparation of EluentsSample Preparation (Fruits and Vegetables)

HPLC Apparatus and ConditionsMS/MS DetectionMethod Transfer ParametersReferencesTrademarks

Experimental Conditions to Analyze Carbamate Pesticides 1


Important Information Go to top READ BEFORE USING ANY RESOURCES PROVIDED HEREIN. For Research Use Only. Not for use in diagnostic procedures. Not for use in clinical investigational procedures. The information provided in this document and the methods included in this package are for information purposes only. Applied Biosystems provides no warranty of performance or suitability for the purpose described herein. Performance on your instrument may be affected by many different variables including (but not limited to): Instrument to instrument variability, instrument tuning, instrument (LC and MS/MS) model variations, reagent variability, differences in preparation techniques, sample matrices, operator abilities, environmental conditions and variability in the matrices employed. Sample data is provided for illustration and example purposes only and represents a small dataset used to verify the method performance on a particular instrument (LC/MS/MS hardware configuration) in our labs. Support for implementation of a similar method in your lab may be available through the Applied Biosystems Field Application Support team, contact your Sales Representative for availability and details. We have provided information about chemicals and reagents used in the development of this package. It is your responsibility to obtain the same or equivalent chemicals to facilitate implementation of such a method, in accordance with any laws requiring licensure, approval, or permits for such chemicals, if and as applicable, and we cannot make any guarantee of performance or suitability for equivalent suppliers, or for consistency in product quality from the suppliers mentioned. The information in no way is intended to be an endorsement of these suppliers. APPLIED BIOSYSTEMS MAKES NO WARRANTIES OF ANY KIND WHATSOEVER, EXPRESS OR IMPLIED, WITH RESPECT TO THE RESOURCES PROVIDED HEREIN, INCLUDING BUT NOT LIMITED TO THE INFORMATION PROVIDED IN THIS DOCUMENT AND THE METHODS PROVIDED HEREIN, INCLUDING BUT NOT LIMITED TO WARRANTIES OF FITNESS FOR A PARTICULAR PURPOSE OR MERCHANTABILITY OR THAT THE RESOURCES ARE NON-INFRINGING. ALL WARRANTIES OF ANY KIND OR NATURE, EXPRESS OR IMPLIED, ARE EXPRESSLY DISCLAIMED. The use of all the resources provided herein is at user's own risk, without recourse to Applied Biosystems. Applied Biosystems has no duty or obligation to maintain or support or perform further development of the methods in any way, or any other duties or obligations with respect thereto.



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Introduction Go to top Thank you for choosing Applied Biosystems LC/MS/MS technology and Cliquid Software. This iMethod Test Kit for Carbamate Pesticides includes method documentation, MS and LC method files, processing method files and report templates, all deployed as a new iMethod Test in your Cliquid Software. Please review the method documentation completely before using the enclosed test. This iMethod Test has been designed by Applied Biosystems to provide the sample preparation and instrument parameters required to accelerate the adoption of this method for routine testing. This method is provided for information purposes only. The performance of this method is not guaranteed due to many different potential variations, including instrument performance, tuning, and maintenance, chemical variability and procedures used, technical experience, sample matrices, and environmental conditions. It is up to the end user to make adjustments to this method to account for slight differences in equipment and/or materials from lab to lab as well as to determine and validate the performance of this method for a given instrument and sample type. Please note that a working knowledge of Analyst Software may be required to do so. This iMethod Test Kit may contain an LC column and associated hardware from a third party manufacturer. We have included this as a convenience so that the conditions used during our development of the test can be more closely duplicated in your laboratory during start-up and testing. Replacement columns are available directly from the manufacturer, and ordering information may be included herein. The suppliers identified in this document and related documents are provided for information purposes only and the list is not intended to be an exhaustive representation of all manufacturers or suppliers of the referenced product. Applied Biosystems/MDS Analytical Technologies makes no warranties or representations as to the performance, fitness or the continued suitability or compliance of a specific product by any of the manufacturers/suppliers referenced herein or the supplier. Applied Biosystems/MDS Analytical Technologies has no responsibility or liability, including indirect or consequential damages or business loss or lost profits, for any use to which the purchaser may put the referenced suppliers products, or for any adverse circumstances arising therefrom. Applied Biosystems does not offer any warranty or guarantee of performance or servicing or repair for any third party components, and any test performance issues which may result from variance of these third party components or servicing or repair issues should be brought to the attention of the third party manufacturer or its representatives in your area for resolution.



Instrumentation Go to top This method has been created for use with the following equipment: API 3200 and 3200 QTRAP LC/MS/MS systems Agilent 1200 Series LC System (for additional information, see HPLC Apparatus and Conditions) Chemicals Go to top 3-Hydroxycarbofuran: C 2H15NO4 Alanycarb: C17H25N3O4S2 1CAS: 16655-82-6 CAS: 83130-01-2

O

OH

ONH

O

CH3

CH3

CH3

N

O

O

N

CH3

CH2

N

S

CH2

CH2

O

O

CH2

CH3

CH3

SCH3

Aldicarb: C7H14N2O2S Aldicarb-sulfone: C7H14N2O4S CAS: 116-06-3 CAS: 1646-88-4

O NH

N CH3O

CH3

CH3SCH3

H

O NH

N CH3O

CH3

CH3SCH3

O

HO



Aldicarb-sulfoxide: C7H14N2O3S Aminocarb: C11H16N2O2 CAS: 1646-87-3 CAS: 2032-59-9

O NH

N CH3O

CH3

CH3SCH3

O

H

O

ONH

N

CH3

CH3CH3

CH3

Bendiocarb: C11H13NO4 Benfuracarb: C20H30N2O5S CAS: 22781-23-3 CAS: 82560-54-1

O

O CH3

CH3

O

O

NH

CH3

O

O

O

N

CH3

CH3

SN

CH3

CH3

CH3

O O CH3 Benomyl: C14H18N4O3 Butocarboxim: C7H14N2O2S CAS: 17804-35-2 CAS: 34681-10-2

N

NH

O CH3

N

NH

OCH3

O

O

ON

CH3

CH3

S CH3NH

CH3

Butocarboxim-sulfoxide: C7H14N2O3S Butoxycarboxim: C7H14N2O4S CAS: 34681-24-8 CAS: 34681-23-7

O

ON

CH3

CH3

S CH3NH

CH3

O

O

ON

CH3

CH3

S CH3NH

CH3

O

O



Carbaryl: C12H11NO2 Carbofuran: C12H15NO3 CAS: 63-25-2 CAS: 1563-66-2

O

ON

CH3

H

O

ONH

CH3

CH3

CH3

O Carbosulfan: C20H32N2O3S Chloropropham: C10H12ClNO2 CAS: 55285-14-8 CAS: 101-21-3

OCH3

CH3

O NS

N

CH3

CH3

CH3

O

Cl

NO

H O CH

CH3

CH3

Dimepiperate: C15H21NOS Dioxacarb: C11H13NO4 CAS: 61432-55-1 CAS: 6988-21-2

NS

CH3CH3

O

OOO

ON

CH3

H

EPTC: C9H19NOS Esprocarb: C15H23NOS CAS: 759-94-4 CAS: 85785-20-2

SCH2 CH3

NCH2

CH2

CH3

CH2CH2

CH3

O

CH2

S C

O

N

CH2CH3

CH

CH3

CH

CH3

CH3



Ethiofencarb: C11H15NO2S Ethiofencarb-sulfone: C11H15NO4S CAS: 29973-13-5 CAS: 53380-23-7

S

ONH

O

S

O

OON

H

O

Ethiofencarb-sulfoxide: C11H15NO3S Fenobucarb: C12H17NO2 CAS: 53380-22-6 CAS: 3766-81-2

S

O

ONH

O

O

CN

CH3

H

O

CH

CH3

CH2 CH3

Fenothiocarb: C13H19NO2S Fenoxycarb: C17H19NO4 CAS: 62850-32-2 CAS: 72490-01-8

N

S

O

O

O

ON

CO

H

O

CH3

Furathiocarb: C18H26N2O5S Iprovalicarb: C18H28N2O3 CAS: 65907-30-4 CAS: 140923-17-7

NOS

N OO

O O

CHCH3 N

C

O

C

H NH C

O CH

CH3

CH3

CH

CH3

CH3

O

HCH3



Isoprocarb: C11H15NO2 Methiocarb: C11H15NO2S CAS: 2631-40-5 CAS: 2032-65-7

NO

CH

CH3

CH3

OCH3

H

SCH3

CH3O

CH3O

NH

CH3

Methiocarb-sulfone: C11H15NO4S Methomyl: C5H10N2O2S CAS: 2179-25-1 CAS: 16752-77-5

SCH3

CH3O

O

NH

CH3

CH3O

O

CO

O

NH

CH3NC

CH3

SCH3

Oxamyl: C7H13N3O3S Phenmedipham: C16H16N2O4 CAS: 23135-22-0 CAS: 13684-63-4

NO

N

O

N

CH3

H

O CH3

CH3

S CH3

CH3

N

H

C

O

O

N

H

C

O

O CH3 Pirimicarb: C11H18N4O2 Promecarb: C12H17NO2 CAS: 23103-98-2 CAS: 2631-37-0

N

N

O

O

N

CH3

CH3CH3

CH3N

CH3

CH3

ON

H

O



Propamocarb: C9H20N2O2 Propoxur: C11H15NO3 CAS: 24579-73-5 CAS: 114-26-1

N NH

O

O

O

ON

CH3

H O CH

CH3

CH3

Pyributicarb: C18H22N2O2S Terbucarb: C17H27NO2 CAS: 88678-67-5 CAS: 1918-11-2

N

N

O

S

CH3

C

CH3

CH3

CH3

O

CH3

OC

O

N

CH3

H

C

CH3CH3

CH3

CH3

C

CH3 CH3

CH3

Thiobencarb: C12H16ClNOS Thiodicarb: C10H18N4O4S3 CAS: 28249-77-6 CAS: 59669-26-0

Cl

CH2S

C

O

NCH2

CH3

CH2CH3

CH3 S

C

CH3

N

O C

O

N CH3

S

N CH3

C

O

O

N

C

CH3

S

CH3



Thiofanox: C9H18N2O2S Thiofanox-sulfone: C9H18N2O4S CAS: 39196-18-4 CAS: 39184-59-3

NH

CH3

O

ON

CH3

CH3 CH3

S

CH3

NH

CH3

O

ON

CH3

CH3 CH3

S CH3

O

O

Thiuram: C6H12N2S4 Triallate: C10H16Cl3NOS CAS: 137-26-8 CAS: 2303-17-5

CH3 N

CH3

C S

S C

N

CH3

CH3

S

S

N C

S

O

CH3

CH3

C

CH3

CH3 CH2 C

Cl

C

Cl

Cl XMC: C10H13NO2 CAS: 2655-14-3

CH3 CH3

O

N

CH3

H

O

Important Note The purchase and use of certain of the chemicals listed below may require the end user to possess any necessary licenses, permits or approvals, if such are required in accordance with local laws and regulations. It is the responsibility of the end user to purchase these chemicals from a licensed supplier, if required in accordance with local laws and regulations. The suppliers and part numbers listed below are for illustrative purposes only and may or may not meet the aforementioned local requirements. Applied Biosystems is not responsible for users compliance with any statute or regulation, or for any permit or approval required for user to implement any iMethod procedure.



Availability Sigma-Aldrich (http://www.sigmaaldrich.com): 3-Hydroxycarbofuran 37896, PESTANAL, analytical standard Aldicarb 33386, PESTANAL, analytical standard Aldicarb-sulfone 33387, PESTANAL, analytical standard Aldicarb-sulfoxide 36784, PESTANAL, analytical standard Aminocarb 45322, PESTANAL, analytical standard Bendiocarb 45336, PESTANAL, analytical standard Benfuracarb 45759, PESTANAL, analytical standard Benomyl 45339, PESTANAL, analytical standard Butocarboxim 36121, PESTANAL, analytical standard Butocarboxim-sulfoxide 45719, PESTANAL, analytical standard Butoxycarboxim 36122, PESTANAL, analytical standard Carbaryl 45367, PESTANAL, analytical standard Carbofuran 45370, PESTANAL, analytical standard Carbosulfan 34300, PESTANAL, analytical standard Chloropropham 45393, PESTANAL, analytical standard Dioxacarb 45454, PESTANAL, analytical standard EPTC 45469, PESTANAL, analytical standard Esprocarb 33898, PESTANAL, analytical standard Ethiofencarb 45475, PESTANAL, analytical standard Ethiofencarb-sulfone 45810, PESTANAL, analytical standard Ethiofencarb-sulfoxide 45811, PESTANAL, analytical standard Fenobucarb 45488, PESTANAL, analytical standard Fenoxycarb 34343, PESTANAL, analytical standard Furathiocarb 45517, PESTANAL, analytical standard Iprovalicarb 33431, PESTANAL, analytical standard Isoprocarb 45541, PESTANAL, analytical standard Methiocarb PS543 Methiocarb-sulfone MET543A Methomyl 36159, PESTANAL, analytical standard Oxamyl 36184, PESTANAL, analytical standard Phenmedipham 36192, PESTANAL, analytical standard Pirimicarb 45627, PESTANAL, analytical standard Promecarb 45634, PESTANAL, analytical standard Propamocarb 45638, PESTANAL, analytical standard Propoxur 45644, PESTANAL, analytical standard Thiobencarb 45687, PESTANAL, analytical standard Thiodicarb 34375, PESTANAL, analytical standard Thiofanox 45314, PESTANAL, analytical standard



Thiofanox-sulfone 45764, PESTANAL, analytical standard Thiuram 45689, PESTANAL, analytical standard Triallate 45695, PESTANAL, analytical standard Dr. Ehrensdorfer/EQ Laboratories (http://www.analytical-standards.com): Carbofuran-3-hydroxy C 11011000, certified Alanycarb XA10063000CY, certified Aldicarb C 10070000, certified Aldicarb-sulfone C 10080000, certified Aldicarb-sulfoxide C 10080500, certified Aminocarb C 10190000, certified Bendiocarb C 10460000, certified Benfuracarb CA10475000, certified Benomyl C 10490000, certified Butocarboxim C 10880000, certified Butocarboxim-sulfoxide C 10890000, certified Butoxycarboxim C 10900000, certified Carbaryl C 10980000, certified Carbofuran C 11010000, certified Carbosulfan CA11030000, certified Chloropropham C 11580000, certified Dimepiperate C 12665000, certified Dioxacarb C 12860000, certified EPTC C 13190000, certified Esprocarb LA13212000AC, certified Ethiofencarb C 13250000, certified Ethiofencarb-sulfone C 13250500, certified Ethiofencarb-sulfoxide C 13251000, certified Fenobucarb C 13485000, certified Fenothiocarb C 13497500, certified Fenoxycarb C 13520000, certified Furathiocarb C 13970000, certified Iprovalicarb C 14371000, certified Isoprocarb C 14450000, certified Methiocarb C 15020500, certified Methiocarb-sulfone C 15020510, certified Methomyl C 15030000, certified Oxamyl C 15780000, certified Phenmedipham 16020000, certified Pirimicarb C 16250000, certified Promecarb C 16350000, certified



Propamocarb (free base) C 16390000, certified Propoxur C 16500000, certified Pyributicarb C 16626000, certified Terbucarb C 17260000, certified Thiobencarb C 17470000, certified Thiodicarb C 17490000, certified Thiofanox C 17500000, certified Thiofanox-sulfone C 17505000, certified Thiuram C 17570000, certified Triallate C 17630000, certified XMC LA17943000CY, certified Wako Pure Chemical Industries (http://www.wako-chem.co.jp/english): Alanycarb 017-15521, for pesticide residue analysis Aldicarb 012-14111, for pesticide residue analysis Bendiocarb 028-11691, for pesticide residue analysis Benfuracarb 023-09551, for pesticide residue analysis Carbaryl (NAC) 148-03831, for pesticide residue analysis Carbofuran 033-16321, for pesticide residue analysis Carbosulfan 49826-76, for pesticide residue analysis Chloropropham (Chloro IPC) 038-08321, for pesticide residue analysis Dimepiperate 047-25171, for pesticide residue analysis EPTC 058-06221, for pesticide residue analysis Esprocarb 059-05891, for pesticide residue analysis Fenobucarb (BPMC) 023-06773, for pesticide residue analysis Fenoxycarb 068-02981, for pesticide residue analysis Furathiocarb 062-03981, for pesticide residue analysis Methiocarb-sulfone 131-12171, for pesticide residue analysis Methomyl 135-10511, for pesticide residue analysis Oxamyl 151-01781, for pesticide residue analysis Propamocarb 161-16731, for pesticide residue analysis Propoxur (PHC) 162-09291, for pesticide residue analysis Pyributicarb 167-16211, for pesticide residue analysis Terbucarb (MBPMC) 132-10901, for pesticide residue analysis Thiobencarb (Benthiocarb) 021-06953, for pesticide residue analysis Thiodicarb 207-11361, for pesticide residue analysis Thiuram 204-11371, for pesticide residue analysis XMC 46001-96, for pesticide residue analysis



HPLC Solvents and Buffers (http://www.sigmaaldrich.com): Water 34877, for HPLC 39253, for LC-MS Methanol 34885, for HPLC 34966, for LC-MS Ammonium formate 17843, puriss. p.a., for HPLC, 99% 55674, puriss. p.a., eluent additive LC-MS Sample Preparation Procedures Go to top Important Note The sample preparation procedures provided are for reference purposes only and represent the procedures used in the development of the method, and procedures used by various other customers, collaborators and Applied Biosystems application scientists. Proper sample preparation procedures are critical to the success of this iMethod Test, and because of the wide variety of equipment and materials available, these preparation procedures can only be offered as examples. Performance of the sample preparation procedures should be verified in your lab with respect to recovery, precision, linearity, and accuracy. All users must be trained and qualified in the performance of the chosen procedure. Various matrices will also have a significant impact on the performance of any of these procedures, and modifications to the procedures or alternate procedures may be needed to successfully prepare the samples for analysis with your chosen sample matrix. Applied Biosystems offers on-site support for the training and development of sample preparation procedures and you may contact your local Applied Biosystems Sales Representative to enquire about these services. Preparation of Eluents Go to top 1 M ammonium formate solution:

Dissolve 63 g of ammonium formate in 1 L HPLC grade water. Eluent A:

Add 5 mL of 1 M ammonium formate solution to 1 L of HPLC grade water.

Eluent B: Add 5 mL of 1 M ammonium formate solution to 1 L of HPLC grade methanol.



Sample Preparation (Fruits and Vegetables) Go to top Based on method by Anastassiadies et al.1 1. Weigh 10 g of blended sample. 2. Add 100 L of internal standard (D5-Atrazine 1 g/mL). 3. Shake vigorously in 10 mL of acetonitrile. 4. Add anhydrous magnesium sulfate (4 g) and sodium chloride (1 g). 5. Vortex immediately to prevent formation of coagulated magnesium sulfate. 6. After shaking for 30 seconds, centrifuge samples at 4300 rpm for 5 minutes. 7. Transfer aliquots (1 mL) of the resulting raw extracts to micro-centrifuge tubes containing

anhydrous magnesium sulfate (150 mg). 8. Mix and centrifuge at 5200 rpm for 1 minute. 9. Adjust an aliquot of 500 L of the combined sample extract to 1 mL with water to give a

solution equivalent to a crop concentration of 0.5 g/mL. Based on method by Klein and Alder et al.2, 3 1. Add water to 5 g or 10 g of a dry or water containing sample to a total volume of 10 mL. 2. Homogenize with 20 mL methanol using an UltraTurrax tissue dispenser for 2 minutes. 3. If necessary filtrate or centrifugate. 4. Add 2 mL NaCl solution (20 g NaCl per 100 mL water) to an aliquot of 6 mL. 5. Soak ChemElut with a 5 mL aliquot of the sample. 6. Elution with 16 mL dichloromethane after 5 minutes. 7. Evaporate to dryness at 40 C. 8. Reconstitute in methanol (0.25 mL) and water (1 mL). 9. Filter through a 0.45 m PTFE filter. Based on method by Lehotay et al.4 1. Homogenize fruit or vegetable using a Molinex mixer or similar apparatus. 2. Add 15 mL of acetonitrile to 15.0 0.05 g of the homogenized sample and sonicate for 2

minutes followed by roller mixing for 5 minutes. 3. Add 6 g of anhydrous magnesium sulphate and 1.5 g of sodium chloride to this mixture

and shake vigorously for 1 minute. 4. Centrifuge at 3000 rpm for 5 minutes. 5. Take 5 mL of the upper layer and add 1.8 g anhydrous magnesium sulphate and 0.3 g of

Bondesil C8 sorbent. 6. Shake the tubes well by hand for 20 seconds. 7. Evaporate to dryness using an Eppendorf Concentrator 5301 or similar apparatus.



8. Reconstitute by dissolving the residue in 100 l of acetonitrile and adding 900 l of water

to make 1 mL of the final extract. 9. Centrifuge this extract for 2 minutes at 12,000 rpm. 10. Transfer the supernatant into an autosampler vial for analysis. HPLC Apparatus and Conditions Go to top Agilent 1100 system Binary pump G1312A (without static mixer) Well-plate autosampler G1367A Micro vacuum degasser G1379B Column oven G1316A Agilent 1200 system Binary pump G1312A (without static mixer) Well-plate autosampler G1367B Micro vacuum degasser G1379B Column oven G1316A Shimadzu Prominence system System controller CBM-20A 2 Isocratic pumps LC-20AD (with semi-micro 100 L mixer) On-line degasser DGU-20A3 Autosampler SIL-20AC Column oven CTO-20AC Column:

Phenomenex Synergi 4 Fusion-RP 80A 50 x 2 mm

Eluent A: H2O + 5 mM ammonium formate

Eluent B: CH3OH + 5 mM ammonium formate



Gradient Profile Step Time (min.) Flow Rate (L/min.) %A %B

0 -5.00 250 80 20 1 0.00 250 80 20 2 8.00 250 10 90 3 14.00 250 10 90 4 15.00 250 80 20

Note: Step 0 is a pre-injection column equilibration step. Column oven temperature: 25 C Injection volume: 10 L MS/MS Detection Go to top Optimized for API 3200 and 3200 QTRAP LC/MS/MS systems TurboIonSpray ion source Positive polarity Source/Gas Parameters CUR: 30 psi IS: 5000 V TEM: 500 C GS1: 40 psi GS2: 60 psi Ihe: On CAD: 5 Compound MRM Parameters and Retention Times MRM pause time: 5 ms Q1 unit resolution Q3 unit resolution



Note: For the Scheduled MRM (sMRM) version of this test, the Scheduled MRM check box

is selected, and the information appearing in the Time column is the retention time of each compound, rather than the dwell time.



The retention times were collected using the Agilent 1200 system and the Shimadzu Prominence system.

Analyte Name Q1 Q3 DP EP CE CXP Agilent RT (min)

Shimadzu RT (min)

3-Hydroxycarbofuran 1 238.1 163.1 42 10 21 4 5 4.13-Hydroxycarbofuran 2 238.1 181.2 42 10 15 2 5 4.1Alanycarb 1 400.1 238.2 15 10 14 3 9.4 9.4Alanycarb 2 400.1 91.1 15 10 40 3 9.4 9.4Aldicarb 1 208.1 116 11 2 11 3 6 5.1Aldicarb 2 208.1 88.9 11 2 20 3 6 5.1Aldicarb-sulfone 1 223.1 86.1 30 10 20 3 2.2 1.7Aldicarb-sulfone 2 223.1 148 30 10 12 3 2.2 1.7Aldicarb-sulfoxide 1 207.1 132.1 21 10 9 3 1.6 1.6Aldicarb-sulfoxide 2 207.1 89.1 21 10 19 3 1.6 1.6Aminocarb 1 209.2 137.1 30 10 32 3 6.7 5.9Aminocarb 2 209.2 152.1 30 10 18 3 6.7 5.9Bendiocarb 1 224.1 109.1 33 10 25 2 6.9 6.1Bendiocarb 2 224.1 167 33 10 12 2 6.9 6.1Benfuracarb 1 411.2 195.1 30 10 30 3 10.1 10.1Benfuracarb 2 411.2 252.1 30 10 19 2 10.1 10.1Benomyl 1 291.1 160 21 10 38 3 9.6 8.9Benomyl 2 291.1 192.1 21 10 18 3 9.6 8.9Butocarboxim 1 191.1 75 13 10 18 3 5.9 4.9Butocarboxim 2 191.1 116 13 10 9 3 5.9 4.9Butocarboxim-sulfoxide 1 207.1 132 22 10 9 3 1.5 1.5Butocarboxim-sulfoxide 2 207.1 75.1 22 10 19 3 1.5 1.5Butoxycarboxim 1 223.1 106 25 10 12 3 2.1 2.1Butoxycarboxim 2 223.1 166 25 10 11 3 2.1 2.1Carbaryl 1 202.1 145.1 31 10 16 3 7.2 6.5Carbaryl 2 202.1 127.1 31 10 39 3 7.2 6.5Carbofuran 1 222.1 165.2 30 10 17 2 6.9 5.7Carbofuran 2 222.1 123 30 10 29 2 6.9 5.7Carbosulfan 1 381.2 118 32 10 27 3 11.5 10.6Carbosulfan 2 381.2 160.2 32 10 20 3 11.5 10.6Chloropropham 1 214.1 172.1 21 10 14 3 8.8 7.7Chloropropham 2 214.1 153.9 21 10 23 3 8.8 7.7Dimepiperate 1 264.1 146.2 22 10 14 3 9.8 9.8Dimepiperate 2 264.1 119 22 10 23 3 9.8 9.8Dioxacarb 1 224 123 21 10 22 3 4.8 3.9Dioxacarb 2 224 167.1 21 10 13 3 4.8 3.9EPTC 1 190.1 128 26 10 15 2 9.2 8.7EPTC 2 190.1 86.1 26 10 17 2 9.2 8.7



Analyte Name Q1 Q3 DP EP CE CXP Agilent RT (min) Shimadzu RT (min)

Esprocarb 1 266.1 91 36 10 35 2 10.1 10.2Esprocarb 2 266.1 65 36 10 79 2 10.1 10.2Ethiofencarb 1 226.1 106.9 21 10 21 2 7.4 6.5Ethiofencarb 2 226.1 164.1 21 10 11 3 7.4 6.5Ethiofencarb-sulfone 1 258.1 107.1 26 10 21 3 4.2 3.3Ethiofencarb-sulfone 2 258.1 201.1 26 10 10 2 4.2 3.3Ethiofencarb-sulfoxide 1 242.1 107.1 23 10 24 3 4.2 3.5Ethiofencarb-sulfoxide 2 242.1 185.1 23 10 12 3 4.2 3.5Fenobucarb 1 208.1 95.2 27 10 19 3 8.3 7.6Fenobucarb 2 208.1 152 27 10 11 3 8.3 7.6Fenothiocarb 1 254.1 72 25 10 28 6 9.2 8.7Fenothiocarb 2 254.1 160.2 25 10 13 3 9.2 8.7Fenoxycarb 1 302.2 88.1 28 10 28 3 9.2 9.2Fenoxycarb 2 302.2 116.2 28 10 16 3 9.2 9.2Furathiocarb 1 383.2 195.2 32 10 24 3 10.1 9.6Furathiocarb 2 383.2 252.2 32 10 17 3 10.1 9.6Iprovalicarb 1 321.2 119 21 10 23 3 9 8.3Iprovalicarb 2 321.2 203.2 21 10 12 2 9 8.3Isoprocarb 1 194.2 95.1 25 10 20 2 7.6 7.1Isoprocarb 2 194.2 137.2 25 10 13 3 7.6 7.1Methiocarb 1 226.1 169.2 25 10 14 3 8.4 7.4Methiocarb 2 226.1 121 25 10 25 3 8.4 7.4Methiocarb-sulfone 1 258.1 122.1 28 10 25 3 5.5 4.9Methiocarb-sulfone 2 258.1 201.2 28 10 13 2 5.5 4.9Methomyl 1 163.1 88.1 15 10 13 3 2.9 2.3Methomyl 2 163.1 106 15 10 13 3 2.9 2.3Oxamyl 1 237.1 72.1 23 4 25 3 2.3 2.3Oxamyl 2 237.1 90.1 23 4 11 3 2.3 2.3Phenmedipham 1 301.1 136 30 10 26 3 8.2 7.6Phenmedipham 2 301.1 168.1 30 10 14 4 8.2 7.6Pirimicarb 1 239.2 72.1 33 10 34 3 7.5 6.7Pirimicarb 2 239.2 182.2 33 10 21 2 7.5 6.7Promecarb 1 208.2 109.2 26 10 21 2 8.5 7.9Promecarb 2 208.2 151.2 26 10 12 3 8.5 7.9Propamocarb 1 189.2 102.2 31 10 24 3 3.2 3.3Propamocarb 2 189.2 73.9 31 10 35 3 3.2 3.3Propoxur 1 210.1 111 21 10 19 3 6.8 5.7Propoxur 2 210.1 168.1 21 10 11 3 6.8 5.7Pyributicarb 1 331.1 181.1 30 10 21 3 10.3 10.3Pyributicarb 2 331.1 108 30 10 40 3 10.3 10.3Terbucarb 1 278.2 166.1 27 10 29 3 9.8 9.3



Analyte Name Q1 Q3 DP EP CE CXP Agilent RT (min) Shimadzu RT (min)

Terbucarb 2 278.2 109 27 10 17 3 9.8 9.3Thiobencarb 1 258.1 125 29 10 25 3 9.6 9.6Thiobencarb 2 258.1 89 29 10 67 2 9.6 9.6Thiodicarb 1 355.1 88.1 20 10 27 3 7.5 7.5Thiodicarb 2 355.1 108 20 10 21 3 7.5 7.5Thiofanox 1 219.1 57.1 15 10 19 2 7.5 6.7Thiofanox 2 219.1 76 15 10 19 6 7.5 6.7Thiofanox-sulfone 1 251.1 57 26 10 21 6 4.7 3.7Thiofanox-sulfone 2 251.1 76.1 26 10 12 3 4.7 3.7Thiuram 1 241 88 21 10 19 3 6.7 6.0Thiuram 2 241 120 21 10 20 3 6.7 6.0Triallate 1 304 143 35 10 34 3 10.4 9.8Triallate 2 304 83.1 35 10 70 3 10.4 9.8XMC 1 180.1 123 21 10 15 3 7.3 7.3XMC 2 180.1 108.1 21 10 37 3 7.3 7.3

Method Transfer Parameters Go to top Important Note The method transfer parameters shown in the table below are provided for the convenience of users with instrumentation different from the instrumentation for which this iMethod test was developed. These parameters are generic and not derived experimentally for this test. In some cases, we provide the iMethod test for a wider combination of instruments and during installation you may be able to install the correct iMethod test for your configuration. The MS and LC portions of the method described herein are for specific instrument configurations, but are generic enough that they can be easily translated for other configurations. Applied Biosystems offers both off and on-site support to assist you in the translation of the iMethod test for your specific configuration. Please contact your local Applied Biosystems Sales Representative for more information about the services available.



LC/MS/MS systems

API

2000 system

QTRAP system

API 3000 system

API 3200 system

3200 QTRAP system

API 4000 system

4000 QTRAP system

API 5000 system

TurboIonSpray ion source parameters CUR 30 30 10 30 30 30 30 30 CAD 5 5 5 5 5 5 5 5 IS (neg) -4200 -4200 -4200 -4200 -4200 -4200 -4200 -4200 IS (pos) 5000 5000 5000 5000 5000 5000 5000 5000 TEM 400 400 400 500 500 500 500 500 GS 1 40 40 NEB: 12 40 40 40 40 40

GS 2 60 60 manual: 7 L/min. 60 60 60 60 60

ihe on on n/a on on on on on Note: For instruments other than the API 3200 or 3200 QTRAP system, begin with the

parameter values appearing in the retention time table on pages 20-22 and transfer them as indicated below (where opt = the parameter value for the instruments used in this method).

LC/MS/MS systems

API

2000 system

QTRAP system

API 3000 system

API 3200 system

3200 QTRAP system

API 4000 system

4000 QTRAP system

API 5000 system

Compound-dependent parameters DP (neg) - opt. - opt. - opt. - opt. - opt. - opt. - 20 - opt. - 20 - opt. - 40 DP (pos) + opt. + opt. + opt. + opt. + opt. + opt. + 20 + opt. + 20 + opt. + 40 FP 360 n/a 160 n/a n/a n/a n/a n/a EP opt. opt. 10 opt. opt. 10 10 10 CE opt. opt. opt. opt. opt. opt. opt. opt. CXP opt. opt. opt. opt. opt. opt. opt. opt. References Go to top 1 M. Anastassiades, S.J. Lehotay, D. Stajnbaher, and F. Schenck: J. AOAC Int. 86(2) (2003)

412431 2 J. Klein and L. Alder: J. AOAC Int. 85(5) (2003) 1015-1037 3 J. Klein et al.: Simultaneous Detection of Determination of residues of approximately 100

pesticides and metabolites in fruit and vegetable by LC/MS/MS (2003) Application Note Applied Biosystems/MDS Sciex

4 S. J. Lethotay, A. Kok, M. Hiemstra, and P. Bodegraven: J. AOAC Int. 88 (2005) 595-614



Trademarks Go to top Applied Biosystems and AB (design) are registered trademarks of Applied Biosystems or its subsidiaries in the US and/or certain other countries. API 2000, API 3000, API 3200, API 4000, API 5000, and IMETHOD are trademarks, and ANALYST, CLIQUID, QTRAP, and TURBOIONSPRAY are registered trademarks of Applied Biosystems/MDS Analytical Technologies, a joint venture between Applied Biosystems and MDS Inc. All other trademarks are the sole property of their respective owners. 2009 Applied Biosystems and MDS Inc. Joint Owners. All Rights Reserved.


Important Information Introduction InstrumentationChemicalsSample Preparation ProceduresPreparation of EluentsSample Preparation (Fruits and Vegetables)

HPLC Apparatus and Conditions MS/MS DetectionMethod Transfer ParametersReferencesTrademarks

fb experimental conditions pesticides carbamates.en

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instrument variability

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instrument tuning

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