FB Experimental Conditions Pesticides Carbamates - en

iMethod Test for Cliquid Software
Experimental Conditions to Analyze

Carbamate Pesticides
Important Information
Introduction
Instrumentation
Chemicals
Sample Preparation Procedures
Preparation of Eluents
Sample Preparation (Fruits and Vegetables)
HPLC Apparatus and Conditions
MS/MS Detection
Method Transfer Parameters
References
Trademarks
Experimental Conditions to Analyze Carbamate Pesticides

1

Important Information
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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
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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
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2

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3

Introduction
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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
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attention of the third party manufacturer or its representatives in your area for resolution.

4

Instrumentation
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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
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3-Hydroxycarbofuran: C12H15NO4
Alanycarb: C17H25N3O4S2
CAS: 16655-82-6
CAS: 83130-01-2
H3C
S
CH3
N
H3C
O
H3C
N
O
H2
C
N
H
C
H2
CH3
C
H2
CH3
O
H2C
CH3
OH
Aldicarb: C7H14N2O2S
Aldicarb-sulfone: C7H14N2O4S
CAS: 116-06-3
CAS: 1646-88-4
H
N
O
H3C
H3C
CH3
O
H
CH3
H
N
O
H3C
O
H3C
CH3
O
H
S
O
CH3

5

Aldicarb-sulfoxide: C7H14N2O3S
Aminocarb: C11H16N2O2
CAS: 1646-87-3
CAS: 2032-59-9
H
N
O
N
H3C
H3C
H3C
CH3
O
CH3
HN
S
O
N
CH3
CH3
CH3
Bendiocarb: C11H13NO4
Benfuracarb: C20H30N2O5S
CAS: 22781-23-3
CAS: 82560-54-1
O
H3C
CH3
N
H
CH3
H3C
CH3
H3C
CH3
CH3
Benomyl: C14H18N4O3
Butocarboxim: C7H14N2O2S
CAS: 17804-35-2
CAS: 34681-10-2
O
N
H
CH3
CH3
O
H3C
N
S
N
H
CH3
N
H
CH3
CH3
Butocarboxim-sulfoxide: C7H14N2O3S
Butoxycarboxim: C7H14N2O4S
CAS: 34681-24-8
CAS: 34681-23-7
CH3
O
H3C
O
CH3
CH3
N
N
H
CH3
CH3
H3C
N
N
H
O
CH3
CH3

6

Carbaryl: C12H11NO2
Carbofuran: C12H15NO3
CAS: 63-25-2
CAS: 1563-66-2
CH3
H3C
N
O
H
N
CH3
H3C
O
Carbosulfan: C20H32N2O3S
Chloropropham: C10H12ClNO2
CAS: 55285-14-8
CAS: 101-21-3
CH3
Cl
S
N
O
N
CH3
O
H3C
CH
CH3
CH3
CH3
H3C
Dimepiperate: C15H21NOS
Dioxacarb: C11H13NO4
CAS: 61432-55-1
CAS: 6988-21-2
H3C
CH3
CH3
O
N
O
O
EPTC: C9H19NOS
Esprocarb: C15H23NOS
CAS: 759-94-4
CAS: 85785-20-2
H3C
CH2
H2C
H2C
H3C
CH2 CH3
H3C
CH2
CH3
CH2
S
C
H2
HC
CH3
CH
CH3
C
O

7

Ethiofencarb: C11H15NO2S
Ethiofencarb-sulfone: C11H15NO4S
CAS: 29973-13-5
CAS: 53380-23-7
O
O
N
H
N
H
O
O
S
O
Ethiofencarb-sulfoxide: C11H15NO3S
Fenobucarb: C12H17NO2
CAS: 53380-22-6
CAS: 3766-81-2
H3C
O
N
N
H
CH3
CH
CH2
CH3
Fenothiocarb: C13H19NO2S
Fenoxycarb: C17H19NO4
CAS: 62850-32-2
CAS: 72490-01-8
O
Furathiocarb: C18H26N2O5S
Iprovalicarb: C18H28N2O3
CAS: 65907-30-4
CAS: 140923-17-7
CH3
S
O
O
N
CH3
CH3
CH CH3
CH N
H
CH3
O CH
N
H
CH3
CH3

8

Isoprocarb: C11H15NO2
Methiocarb: C11H15NO2S
CAS: 2631-40-5
CAS: 2032-65-7
CH3
CH3
CH3
CH CH3
H3C
N
H
CH3
Methiocarb-sulfone: C11H15NO4S
Methomyl: C5H10N2O2S
CAS: 2179-25-1
CAS: 16752-77-5
CH3 O
S
O
H3C
N
H
CH3
O
S
H3C
N
C
CH3
CH3
CH3
C
O
N
H
CH3
Oxamyl: C7H13N3O3S
Phenmedipham: C16H16N2O4
CAS: 23135-22-0
CAS: 13684-63-4
CH3
H3C
CH3
N C
N
H
CH3
Pirimicarb: C11H18N4O2
Promecarb: C12H17NO2
CAS: 23103-98-2
CAS: 2631-37-0
H3 C
C
O
CH3
O
O
N
H3C
CH3
N
H3 C
CH3
CH3
CH3

9

Propamocarb: C9H20N2O2
Propoxur: C11H15NO3
CAS: 24579-73-5
CAS: 114-26-1
CH3
N
H
O CH CH3
CH3
Pyributicarb: C18H22N2O2S
Terbucarb: C17H27NO2
CAS: 88678-67-5
CAS: 1918-11-2
CH3
C
CH3
O
H3C
H3C
CH3
H3C
N
N
O
CH3
CH3
C
CH3
CH3
CH3
CH3
CH3
Thiobencarb: C12H16ClNOS
Thiodicarb: C10H18N4O4S3
CAS: 28249-77-6
CAS: 59669-26-0
H3C
S
C
H3C
N
O
C
N
CH3
CH3
H3C
H2C
H3C
C
N
CH2
C
CH3
C
CH2
Cl
H3C

10

Thiofanox: C9H18N2O2S
Thiofanox-sulfone: C9H18N2O4S
CAS: 39196-18-4
CAS: 39184-59-3
O
CH3
O
H3C
H3C
N
H
S
O
H3C
O
O
H3C
CH3
CH3
CH3
Thiuram: C6H12N2S4
Triallate: C10H16Cl3NOS
CAS: 137-26-8
CAS: 2303-17-5
CH3
CH3
H3C
N
C
H3C
CH3
N
H
CH3
H3C
CH3
H3C
C
S
C
CH3
C
S
CH2
Cl
Cl
C
Cl
XMC: C10H13NO2
CAS: 2655-14-3
O
H3C
N
H
H3C
CH3
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.
11

Availability
Sigma-Aldrich (http://www.sigmaaldrich.com):
3-Hydroxycarbofuran
Aldicarb
Aldicarb-sulfone
Aldicarb-sulfoxide
Aminocarb
Bendiocarb
Benfuracarb
Benomyl
Butocarboxim
Butocarboxim-sulfoxide
Butoxycarboxim
Carbaryl
Carbofuran
Carbosulfan
Chloropropham
Dioxacarb
EPTC
Esprocarb
Ethiofencarb
Ethiofencarb-sulfone
Ethiofencarb-sulfoxide
Fenobucarb
Fenoxycarb
Furathiocarb
Iprovalicarb
Isoprocarb
Methiocarb
Methiocarb-sulfone
Methomyl
Oxamyl
Phenmedipham
Pirimicarb
Promecarb
Propamocarb
Propoxur
Thiobencarb
Thiodicarb
Thiofanox
37896, PESTANAL, analytical standard

PS543
MET543A

12

Thiofanox-sulfone
Thiuram
Triallate

Dr. Ehrensdorfer/EQ Laboratories (http://www.analytical-standards.com):

Carbofuran-3-hydroxy
Alanycarb
Aldicarb
Aldicarb-sulfone
Aldicarb-sulfoxide
Aminocarb
Bendiocarb
Benfuracarb
Benomyl
Butocarboxim
Butocarboxim-sulfoxide
Butoxycarboxim
Carbaryl
Carbofuran
Carbosulfan
Chloropropham
Dimepiperate
Dioxacarb
EPTC
Esprocarb
Ethiofencarb
Ethiofencarb-sulfone
Ethiofencarb-sulfoxide
Fenobucarb
Fenothiocarb
Fenoxycarb
Furathiocarb
Iprovalicarb
Isoprocarb
Methiocarb
Methiocarb-sulfone
Methomyl
Oxamyl
Phenmedipham
Pirimicarb
Promecarb
C 11011000, certified
XA10063000CY, certified
CA10475000, certified
CA11030000, certified
LA13212000AC, certified
16020000, certified

13

Propamocarb (free base)
Propoxur
Pyributicarb
Terbucarb
Thiobencarb
Thiodicarb
Thiofanox
Thiofanox-sulfone
Thiuram
Triallate
XMC
LA17943000CY, certified
Wako Pure Chemical Industries (http://www.wako-chem.co.jp/english):

Alanycarb
Aldicarb
Bendiocarb
Benfuracarb
Carbaryl (NAC)
Carbofuran
Carbosulfan
Chloropropham (Chloro IPC)
Dimepiperate
EPTC
Esprocarb
Fenobucarb (BPMC)
Fenoxycarb
Furathiocarb
Methiocarb-sulfone
Methomyl
Oxamyl
Propamocarb
Propoxur (PHC)
Pyributicarb
Terbucarb (MBPMC)
Thiobencarb (Benthiocarb)
Thiodicarb
Thiuram
XMC
017-15521, for pesticide residue analysis


14

HPLC Solvents and Buffers (http://www.sigmaaldrich.com):
Water
Methanol
Ammonium formate
34877, for HPLC

39253, for LC-MS
34885, for HPLC
34966, for LC-MS
17843, puriss. p.a., for HPLC, 99%
55674, puriss. p.a., eluent additive LC-MS
Sample Preparation Procedures

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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
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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.

15

Sample Preparation (Fruits and Vegetables)
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Based on method by Anastassiadies et al.1
1.
2.
3.
4.
5.
6.
7.
8.
9.
Weigh 10 g of blended sample.

Add 100 L of internal standard (D5-Atrazine 1 g/mL).
Shake vigorously in 10 mL of acetonitrile.
Add anhydrous magnesium sulfate (4 g) and sodium chloride (1 g).
Vortex immediately to prevent formation of coagulated magnesium sulfate.
After shaking for 30 seconds, centrifuge samples at 4300 rpm for 5 minutes.
Transfer aliquots (1 mL) of the resulting raw extracts to micro-centrifuge tubes containing
anhydrous magnesium sulfate (150 mg).
Mix and centrifuge at 5200 rpm for 1 minute.
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.
2.
3.
4.
5.
6.
7.
8.
9.
Add water to 5 g or 10 g of a dry or water containing sample to a total volume of 10 mL.

Homogenize with 20 mL methanol using an UltraTurrax tissue dispenser for 2 minutes.
If necessary filtrate or centrifugate.
Add 2 mL NaCl solution (20 g NaCl per 100 mL water) to an aliquot of 6 mL.
Soak ChemElut with a 5 mL aliquot of the sample.
Elution with 16 mL dichloromethane after 5 minutes.
Evaporate to dryness at 40 C.
Reconstitute in methanol (0.25 mL) and water (1 mL).
Filter through a 0.45 m PTFE filter.
Based on method by Lehotay et al.4

1.
2.
3.
4.
5.
6.
7.
Homogenize fruit or vegetable using a Molinex mixer or similar apparatus.

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.
Add 6 g of anhydrous magnesium sulphate and 1.5 g of sodium chloride to this mixture
and shake vigorously for 1 minute.
Centrifuge at 3000 rpm for 5 minutes.
Take 5 mL of the upper layer and add 1.8 g anhydrous magnesium sulphate and 0.3 g of
Bondesil C8 sorbent.
Shake the tubes well by hand for 20 seconds.
Evaporate to dryness using an Eppendorf Concentrator 5301 or similar apparatus.

16

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
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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

17

Gradient Profile
Step
Time (min.)
0
1
2
3
4
-5.00
0.00
8.00
14.00
15.00
Flow Rate (L/min.)

250
250
250
250
250
%A
%B
80
80
10
10
80
20
20
90
90
20
Note: Step 0 is a pre-injection column equilibration step.

Column oven temperature: 25 C
Injection volume: 10 L
MS/MS Detection
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Optimized for API 3200 and 3200 QTRAP LC/MS/MS systems
TurboIonSpray ion source
Positive polarity
Source/Gas Parameters
CUR:
IS:
TEM:
GS1:
GS2:
Ihe:
CAD:
30 psi
5000 V
500 C
40 psi
60 psi
On
5
Compound MRM Parameters and Retention Times

MRM pause time: 5 ms
Q1 unit resolution
Q3 unit resolution

18
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.

19

The retention times were collected using the Agilent 1200 system and the Shimadzu
Prominence system.
Analyte Name
Q1
3-Hydroxycarbofuran 1
3-Hydroxycarbofuran 2
Alanycarb 1
Alanycarb 2
Aldicarb 1
Aldicarb 2
Aldicarb-sulfone 1
Aldicarb-sulfone 2
Aldicarb-sulfoxide 1
Aldicarb-sulfoxide 2
Aminocarb 1
Aminocarb 2
Bendiocarb 1
Bendiocarb 2
Benfuracarb 1
Benfuracarb 2
Benomyl 1
Benomyl 2
Butocarboxim 1
Butocarboxim 2
Butocarboxim-sulfoxide 1
Butocarboxim-sulfoxide 2
Butoxycarboxim 1
Butoxycarboxim 2
Carbaryl 1
Carbaryl 2
Carbofuran 1
Carbofuran 2
Carbosulfan 1
Carbosulfan 2
Chloropropham 1
Chloropropham 2
Dimepiperate 1
Dimepiperate 2
Dioxacarb 1
Dioxacarb 2
EPTC 1
EPTC 2
238.1
238.1
400.1
400.1
208.1
208.1
223.1
223.1
207.1
207.1
209.2
209.2
224.1
224.1
411.2
411.2
291.1
291.1
191.1
191.1
207.1
207.1
223.1
223.1
202.1
202.1
222.1
222.1
381.2
381.2
214.1
214.1
264.1
264.1
224
224
190.1
190.1
Q3
163.1
181.2
238.2
91.1
116
88.9
86.1
148
132.1
89.1
137.1
152.1
109.1
167
195.1
252.1
160
192.1
75
116
132
75.1
106
166
145.1
127.1
165.2
123
118
160.2
172.1
153.9
146.2
119
123
167.1
128
86.1
DP
42
42
15
15
11
11
30
30
21
21
30
30
33
33
30
30
21
21
13
13
22
22
25
25
31
31
30
30
32
32
21
21
22
22
21
21
26
26
EP
10
10
10
10
2
2
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
CE
21
15
14
40
11
20
20
12
9
19
32
18
25
12
30
19
38
18
18
9
9
19
12
11
16
39
17
29
27
20
14
23
14
23
22
13
15
17
CXP
4
2
3
3
3
3
3
3
3
3
3
3
2
2
3
2
3
3
3
3
3
3
3
3
3
3
2
2
3
3
3
3
3
3
3
3
2
2
Agilent
RT (min)
5
5
9.4
9.4
6
6
2.2
2.2
1.6
1.6
6.7
6.7
6.9
6.9
10.1
10.1
9.6
9.6
5.9
5.9
1.5
1.5
2.1
2.1
7.2
7.2
6.9
6.9
11.5
11.5
8.8
8.8
9.8
9.8
4.8
4.8
9.2
9.2
Shimadzu
RT (min)
4.1
4.1
9.4
9.4
5.1
5.1
1.7
1.7
1.6
1.6
5.9
5.9
6.1
6.1
10.1
10.1
8.9
8.9
4.9
4.9
1.5
1.5
2.1
2.1
6.5
6.5
5.7
5.7
10.6
10.6
7.7
7.7
9.8
9.8
3.9
3.9
8.7
8.7

20

Analyte Name
Q1
Esprocarb 1
Esprocarb 2
Ethiofencarb 1
Ethiofencarb 2
Ethiofencarb-sulfone 1
Ethiofencarb-sulfone 2
Ethiofencarb-sulfoxide 1
Ethiofencarb-sulfoxide 2
Fenobucarb 1
Fenobucarb 2
Fenothiocarb 1
Fenothiocarb 2
Fenoxycarb 1
Fenoxycarb 2
Furathiocarb 1
Furathiocarb 2
Iprovalicarb 1
Iprovalicarb 2
Isoprocarb 1
Isoprocarb 2
Methiocarb 1
Methiocarb 2
Methiocarb-sulfone 1
Methiocarb-sulfone 2
Methomyl 1
Methomyl 2
Oxamyl 1
Oxamyl 2
Phenmedipham 1
Phenmedipham 2
Pirimicarb 1
Pirimicarb 2
Promecarb 1
Promecarb 2
Propamocarb 1
Propamocarb 2
Propoxur 1
Propoxur 2
Pyributicarb 1
Pyributicarb 2
Terbucarb 1
266.1
266.1
226.1
226.1
258.1
258.1
242.1
242.1
208.1
208.1
254.1
254.1
302.2
302.2
383.2
383.2
321.2
321.2
194.2
194.2
226.1
226.1
258.1
258.1
163.1
163.1
237.1
237.1
301.1
301.1
239.2
239.2
208.2
208.2
189.2
189.2
210.1
210.1
331.1
331.1
278.2
Q3
91
65
106.9
164.1
107.1
201.1
107.1
185.1
95.2
152
72
160.2
88.1
116.2
195.2
252.2
119
203.2
95.1
137.2
169.2
121
122.1
201.2
88.1
106
72.1
90.1
136
168.1
72.1
182.2
109.2
151.2
102.2
73.9
111
168.1
181.1
108
166.1
DP
36
36
21
21
26
26
23
23
27
27
25
25
28
28
32
32
21
21
25
25
25
25
28
28
15
15
23
23
30
30
33
33
26
26
31
31
21
21
30
30
27
EP
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
4
4
10
10
10
10
10
10
10
10
10
10
10
10
10
CE
35
79
21
11
21
10
24
12
19
11
28
13
28
16
24
17
23
12
20
13
14
25
25
13
13
13
25
11
26
14
34
21
21
12
24
35
19
11
21
40
29
CXP
2
2
2
3
3
2
3
3
3
3
6
3
3
3
3
3
3
2
2
3
3
3
3
2
3
3
3
3
3
4
3
2
2
3
3
3
3
3
3
3
3
Agilent
RT (min)
10.1
10.1
7.4
7.4
4.2
4.2
4.2
4.2
8.3
8.3
9.2
9.2
9.2
9.2
10.1
10.1
9
9
7.6
7.6
8.4
8.4
5.5
5.5
2.9
2.9
2.3
2.3
8.2
8.2
7.5
7.5
8.5
8.5
3.2
3.2
6.8
6.8
10.3
10.3
9.8
Shimadzu
RT (min)
10.2
10.2
6.5
6.5
3.3
3.3
3.5
3.5
7.6
7.6
8.7
8.7
9.2
9.2
9.6
9.6
8.3
8.3
7.1
7.1
7.4
7.4
4.9
4.9
2.3
2.3
2.3
2.3
7.6
7.6
6.7
6.7
7.9
7.9
3.3
3.3
5.7
5.7
10.3
10.3
9.3

21

Analyte Name
Q1
Terbucarb 2
Thiobencarb 1
Thiobencarb 2
Thiodicarb 1
Thiodicarb 2
Thiofanox 1
Thiofanox 2
Thiofanox-sulfone 1
Thiofanox-sulfone 2
Thiuram 1
Thiuram 2
Triallate 1
Triallate 2
XMC 1
XMC 2
278.2
258.1
258.1
355.1
355.1
219.1
219.1
251.1
251.1
241
241
304
304
180.1
180.1
Q3
109
125
89
88.1
108
57.1
76
57
76.1
88
120
143
83.1
123
108.1
DP
27
29
29
20
20
15
15
26
26
21
21
35
35
21
21
EP
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
CE
17
25
67
27
21
19
19
21
12
19
20
34
70
15
37
CXP
3
3
2
3
3
2
6
6
3
3
3
3
3
3
3
Agilent
RT (min)
9.8
9.6
9.6
7.5
7.5
7.5
7.5
4.7
4.7
6.7
6.7
10.4
10.4
7.3
7.3
Shimadzu
RT (min)
9.3
9.6
9.6
7.5
7.5
6.7
6.7
3.7
3.7
6.0
6.0
9.8
9.8
7.3
7.3
Method Transfer Parameters

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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.

22

LC/MS/MS systems
API
QTRAP
2000
system
system
API
3000
system
API
3200
system
3200
QTRAP
system
API
4000
system
4000
QTRAP
system
API
5000
system
TurboIonSpray ion source parameters

CUR
CAD
IS (neg)
IS (pos)
TEM
GS 1
30
5
-4200
5000
400
40
30
5
-4200
5000
400
40
GS 2
60
60
ihe
on
on
10
5
-4200
5000
400
NEB: 12
manual:
7 L/min.
n/a
30
5
-4200
5000
500
40
30
5
-4200
5000
500
40
30
5
-4200
5000
500
40
30
5
-4200
5000
500
40
30
5
-4200
5000
500
40
60
60
60
60
60
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
QTRAP
2000
system
system
API
3000
system
API
3200
system
3200
QTRAP
system
API
4000
system
4000
QTRAP
system
API
5000
system
- opt. - 20
+ opt. + 20
n/a
10
opt.
opt.
- opt. - 20
+ opt. + 20
n/a
10
opt.
opt.
- opt. - 40
+ opt. + 40
n/a
10
opt.
opt.
Compound-dependent parameters
DP (neg)
DP (pos)
FP
EP
CE
CXP
- opt.
+ opt.
360
opt.
opt.
opt.
- opt.
+ opt.
n/a
opt.
opt.
opt.
- opt.
+ opt.
160
10
opt.
opt.
- opt.
+ opt.
n/a
opt.
opt.
opt.
- opt.
+ opt.
n/a
opt.
opt.
opt.
References
Go to top
1
2
3
M. Anastassiades, S.J. Lehotay, D. Stajnbaher, and F. Schenck: J. AOAC Int. 86(2) (2003)
412431
J. Klein and L. Alder: J. AOAC Int. 85(5) (2003) 1015-1037
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
S. J. Lethotay, A. Kok, M. Hiemstra, and P. Bodegraven: J. AOAC Int. 88 (2005) 595-614

23

Trademarks
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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.

24

FB Experimental Conditions Pesticides Carbamates - en

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FB Experimental Conditions Pesticides Carbamates - en

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iMethod Test for Cliquid Software

Experimental Conditions to Analyze

Experimental Conditions to Analyze Carbamate Pesticides

iMethod Test for Cliquid Software

iMethod Test for Cliquid Software

Experimental Conditions to Analyze Carbamate Pesticides

iMethod Test for Cliquid Software

Experimental Conditions to Analyze Carbamate Pesticides

iMethod Test for Cliquid Software

Experimental Conditions to Analyze Carbamate Pesticides

iMethod Test for Cliquid Software

Experimental Conditions to Analyze Carbamate Pesticides

iMethod Test for Cliquid Software

Experimental Conditions to Analyze Carbamate Pesticides

iMethod Test for Cliquid Software

Experimental Conditions to Analyze Carbamate Pesticides

iMethod Test for Cliquid Software

Experimental Conditions to Analyze Carbamate Pesticides

iMethod Test for Cliquid Software

Experimental Conditions to Analyze Carbamate Pesticides

iMethod Test for Cliquid Software

iMethod Test for Cliquid Software

37896, PESTANAL, analytical standard

Experimental Conditions to Analyze Carbamate Pesticides

iMethod Test for Cliquid Software

45764, PESTANAL, analytical standard

Dr. Ehrensdorfer/EQ Laboratories (http://www.analytical-standards.com):

Experimental Conditions to Analyze Carbamate Pesticides

iMethod Test for Cliquid Software

Wako Pure Chemical Industries (http://www.wako-chem.co.jp/english):

017-15521, for pesticide residue analysis

Experimental Conditions to Analyze Carbamate Pesticides

iMethod Test for Cliquid Software

34877, for HPLC

Sample Preparation Procedures

Experimental Conditions to Analyze Carbamate Pesticides

iMethod Test for Cliquid Software

Weigh 10 g of blended sample.

Based on method by Klein and Alder et al.2, 3

Add water to 5 g or 10 g of a dry or water containing sample to a total volume of 10 mL.

Based on method by Lehotay et al.4

Homogenize fruit or vegetable using a Molinex mixer or similar apparatus.

Experimental Conditions to Analyze Carbamate Pesticides

iMethod Test for Cliquid Software

Experimental Conditions to Analyze Carbamate Pesticides

iMethod Test for Cliquid Software

Flow Rate (L/min.)

Note: Step 0 is a pre-injection column equilibration step.

Compound MRM Parameters and Retention Times

Experimental Conditions to Analyze Carbamate Pesticides

iMethod Test for Cliquid Software

Experimental Conditions to Analyze Carbamate Pesticides

iMethod Test for Cliquid Software

Experimental Conditions to Analyze Carbamate Pesticides

iMethod Test for Cliquid Software

Experimental Conditions to Analyze Carbamate Pesticides

iMethod Test for Cliquid Software

Method Transfer Parameters

Experimental Conditions to Analyze Carbamate Pesticides

iMethod Test for Cliquid Software

TurboIonSpray ion source parameters

Experimental Conditions to Analyze Carbamate Pesticides

iMethod Test for Cliquid Software