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Pesticide Residue Analysis in Kale by LC-MS/MS on Ultra Aqueous C18

LC_FF0516
PeakstR (min)MRM 1MRM 2
1.Methamidophos1.27142.1 / 94.1142.1 / 112.2
2.Acephate1.78184.1 / 125.1184.1 / 95.1
3.Propamocarb2.65189.2 / 102.0189.2 / 144.2
4.Omethoate2.94214.1 / 125.2214.1 / 155.1
5.Aldicarb sulfone3.45223.2 / 148.0223.2 / 76.2
6.Aldicarb sulfoxide3.71207.2 / 132.1207.2 / 89.1
7.Pymetrozine3.82218.1 / 105.0218.1 / 78.2
8.Oxamyl3.90237.1 / 71.9237.1 / 90.1
9.Methomyl4.02163.1 / 88.1163.1 / 106.2
10.Monocrotophos4.38224.1 / 127.1224.1 / 98.1
11.Dimethoate4.81230.1 / 125.2230.1 / 171.2
12.Mevinphos E4.99225.2 / 193.3225.2 / 127.2
13.Thiabendazole4.99202.2 / 175.0202.2 / 131.2
14.Imidacloprid5.02256.3 / 209.1256.3 / 175.2
15.Mevinphos Z5.43225.1 / 193.2225.1 / 127.1
16.Aldicarb5.55208.2 / 116.2208.2 / 89.1
17.Carbetamide5.73237.1 / 192.0237.1 / 118.1
18.Imazethapyr5.90290.1 / 245.2290.1 / 177.3
19.Thidiazuron5.93221.2 / 102.0221.2 / 128.1
20.Thiophanate methyl5.96343.2 / 151.1343.2 / 93.1
21.Propoxur5.99210.2 / 168.1210.2 / 111.2
22.Bendiocarb6.00224.1 / 109.2224.1 / 167.2
23.Dichlorvos6.01220.9 / 109.2220.9 / 95.0
24.Carbofuran6.09222.3 / 165.2222.3 / 123.1
25.Pirimicarb6.15239.2 / 72.2239.2 / 182.2
26.Carbaryl6.32202.3 / 127.1202.3 / 117.2
27.Imazalil6.40297.1 / 159.0297.1 / 173.1
28.Isoprocarb6.53194.3 / 95.2194.3 / 137.3
29.Metalaxyl6.72280.4 / 192.3280.4 / 160.2
30.Metalaxyl-m6.72280.4 / 220.3280.4 / 192.1
31.Atrazine6.75216.2 / 174.3216.2 / 132.1
32.Atrazine-d5 (IS)6.77221.1 / 179.0221.1 / 101.2
33.Isoproturon6.86207.2 / 72.3207.2 / 134.3
34.Azinphos-methyl6.96318.2 / 160.0318.2 / 132.1
35.Diuron6.97233.1 / 72.1233.1 / 160.0
36.Phosmet6.97318.1 / 160.2318.1 / 133.0
37.Demeton-O6.98259.0 / 89.1259.0 / 61.2
38.Demeton-S6.98259.2 / 88.9259.2 / 61.1
39.Nuarimol7.08315.0 / 252.1315.0 / 81.0
40.Propanil7.11218.2 / 162.0218.2 / 127.0
41.Azoxystrobin7.12404.3 / 372.3404.3 / 344.0
42.Malathion7.13331.1 / 127.1331.1 / 99.1
43.Methiocarb7.14226.1 / 169.1226.1 / 121.1
44.Chlorpropham7.20214.1 / 154.0214.1 / 126.1
45.Linuron7.20249.2 / 160.1249.2 / 182.1
46.Crotoxyphos7.21332.2 / 211.2332.2 / 167.2
47.Promecarb7.21208.8 / 109.2208.8 / 151.3
48.Propetamphos7.22282.1 / 138.0282.1 / 110.2
49.Boscalid7.25343.2 / 307.2343.2 / 140.0
50.Triadimefon7.26294.3 / 197.1294.3 / 69.2
51.Triadimenol7.35296.3 / 70.2296.3 / 227.1
52.Fenhexamid7.40302.1 / 97.1302.1 / 55.0
PeakstR (min)MRM 1MRM 2
53.Myclobutanil7.43289.3 / 70.2289.3 / 124.9
54.Dichlofluanid7.44332.9 / 224.0332.9 / 123.1
55.Triazophos7.48314.1 / 162.0314.1 / 119.2
56.Alachlor7.60270.2 / 238.1270.2 / 162.2
57.Fenarimol7.61331.0 / 268.0331.0 / 81.0
58.Iprodione7.66330.3 / 245.2332.3 / 247.0
59.Ethoprop7.70243.1 / 131.0243.1 / 173.0
60.Parathion7.77292.1 / 236.0292.1 / 140.1
61.Fenamiphos7.83304.4 / 217.2304.4 / 202.0
62.Diflubenzuron7.85311.1 / 158.2311.1 / 141.1
63.Fenoxycarb7.87302.1 / 88.0302.1 / 116.1
64.Etaconazole isomer 17.89328.2 / 159.1328.2 / 123.0
65.Fenbuconazole7.89337.3 / 125.3337.3 / 70.3
66.Kresoxim-methyl7.90314.2 / 115.9314.2 / 131.0
67.Tolyfluanid8.00364.0 / 238.0364.0 / 137.1
68.Etaconazole isomer 28.01328.3 / 159.2328.3 / 123.1
69.Fenthion8.06279.1 / 169.1279.1 / 105.1
70.Quinalphos8.07299.3 / 243.1299.3 / 163.2
71.Cyprodinil8.16226.1 / 93.3226.1 / 77.1
72.Tebuconazole8.24308.3 / 70.1308.3 / 125.1
73.Chlorfenvinphos8.32359.2 / 155.1359.2 / 99.2
74.Diazinon8.34305.2 / 169.3305.2 / 153.1
75.Pirimiphos methyl8.35306.1 / 164.3306.1 / 108.1
76.Phosalone8.38368.1 / 182.1368.1 / 138.0
77.Diazinon-d10 (IS)8.39315.3 / 170.1315.3 / 154.1
78.Coumaphos8.46363.1 / 227.2363.1 / 211.1
79.Propiconazole isomer 18.60342.3 / 159.0342.3 / 69.3
80.Pyraclostrobin8.61388.0 / 164.2388.0 / 194.3
81.Chlorpyrifos methyl8.72323.9 / 125.0323.9 / 291.8
82.Propiconazole isomer 28.77342.4 / 159.1342.4 / 69.4
83.Dialifos8.81394.3 / 208.0394.3 / 187.0
84.Prochloraz9.01376.1 / 308.1376.1 / 266.0
85.Indoxacarb9.04528.6 / 218.0528.6 / 150.2
86.Trifloxystrobin9.18409.4 / 186.0409.4 / 145.1
87.Spinosyn A9.58733.1 / 142.4733.1 / 98.4
88.Difenoconazole isomer 19.60406.3 / 251.1408.2 / 253.1
89.Triflumizole9.79346.2 / 278.2346.2 / 73.1
90.Difenoconazole isomer 29.85406.4 / 251.2408.3 / 253.2
91.Ethion10.20385.3 / 199.0385.3 / 171.0
92.Spinosyn D10.38746.8 / 142.4746.8 / 98.3
93.Chlorpyrifos10.40350.0 / 198.0350.0 / 97.0
94.Pendimethalin10.47282.3 / 212.2282.3 / 194.3
95.Emamectin B1a benzoate10.48887.2 / 158.3887.2 / 126.3
96.Propargite10.61368.4 / 175.1368.4 / 231.2
97.Fenpropathrin10.67350.3 / 125.0350.3 / 97.4
98.Flufenoxuron10.72489.5 / 158.2489.5 / 141.1
99.Lambda cyhalothrin10.72467.4 / 225.1467.4 / 181.0
100.Deltamethrin10.78523.3 / 280.9523.3 / 181.0
101.trans-Permethrin10.90408.4 / 183.3408.4 / 153.2
102.Leptophos10.92413.2 / 171.0413.2 / 77.1
103.cis-Permethrin10.95408.5 / 183.1408.5 / 153.2
104.Bifenthrin10.98440.3 / 181.2440.3 / 166.2
Isomers were designated 1 or 2 by elution order
ColumnUltra Aqueous C18 (cat.# 9178312)
Dimensions:100 mm x 2.1 mm ID
Particle Size:3 µm
Pore Size:100 Å
Temp.:50 °C
SampleKale extract diluted 10x in mobile phase A
Diluent:Mobile phase A
Conc.:10 ng/mL
Inj. Vol.:20 µL
Mobile Phase
A:Water + 0.1% formic acid + 4 mM ammonium formate
B:Methanol + 0.1% formic acid + 4 mM ammonium formate
Time (min)Flow (mL/min)%A%B
0.000.59010
1.500.59010
6.000.53070
9.000.53070
10.000.50100
12.000.50100
12.010.59010
15.000.59010
DetectorABSCIEX MS/MS
Model #:API 4000
Ion Source:TurboIonSpray®
Ion Mode:ESI+
Ion Spray Voltage:5.5 kV
Curtain Gas:30 psi (206.8 kPa)
Gas 1:40 psi (275.8 kPa)
Gas 2:45 psi (310.3 kPa)
CAD:10 psi (68.9 kPa)
Source Temp.:450 °C
Mode:Scheduled MRM
MRM Detection Window:45 sec
Target Scan Time:0.33 sec
InstrumentAPI LC-MS/MS
NotesThe AOAC QuEChERS method was used. 15 mL of acetonitrile with 1% acetic acid (v/v) was added to 15 g of fortified homogenized kale. Q-sep AOAC buffering extraction salts (cat.# 26237) containing 6 g MgSO4 and 1.5 g sodium acetate were added. Following 1 minute of manual shaking, samples were centrifuged for 5 minutes at 3,000 U/min with a Q-sep 3000 centrifuge (cat.# 26230). The top acetonitrile layer was removed to a clean vial. A Restek Q-sep dSPE tube, cat.# 26126, containing 300 mg PSA, 150 mg GCB, and 900 mg MgSO4 was used to process 6 mL of kale extract. The tube was shaken for 2 minutes and centrifuged for 5 minutes at 3,000 U/min. The sample was diluted 10-fold in mobile phase A before injection.