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Peaks | tR (min) | MRM 1 | MRM 2 | |
---|---|---|---|---|
1. | Methamidophos | 1.27 | 142.1 / 94.1 | 142.1 / 112.2 |
2. | Acephate | 1.78 | 184.1 / 125.1 | 184.1 / 95.1 |
3. | Propamocarb | 2.65 | 189.2 / 102.0 | 189.2 / 144.2 |
4. | Omethoate | 2.94 | 214.1 / 125.2 | 214.1 / 155.1 |
5. | Aldicarb sulfone | 3.45 | 223.2 / 148.0 | 223.2 / 76.2 |
6. | Aldicarb sulfoxide | 3.71 | 207.2 / 132.1 | 207.2 / 89.1 |
7. | Pymetrozine | 3.82 | 218.1 / 105.0 | 218.1 / 78.2 |
8. | Oxamyl | 3.90 | 237.1 / 71.9 | 237.1 / 90.1 |
9. | Methomyl | 4.02 | 163.1 / 88.1 | 163.1 / 106.2 |
10. | Monocrotophos | 4.38 | 224.1 / 127.1 | 224.1 / 98.1 |
11. | Dimethoate | 4.81 | 230.1 / 125.2 | 230.1 / 171.2 |
12. | Mevinphos E | 4.99 | 225.2 / 193.3 | 225.2 / 127.2 |
13. | Thiabendazole | 4.99 | 202.2 / 175.0 | 202.2 / 131.2 |
14. | Imidacloprid | 5.02 | 256.3 / 209.1 | 256.3 / 175.2 |
15. | Mevinphos Z | 5.43 | 225.1 / 193.2 | 225.1 / 127.1 |
16. | Aldicarb | 5.55 | 208.2 / 116.2 | 208.2 / 89.1 |
17. | Carbetamide | 5.73 | 237.1 / 192.0 | 237.1 / 118.1 |
18. | Imazethapyr | 5.90 | 290.1 / 245.2 | 290.1 / 177.3 |
19. | Thidiazuron | 5.93 | 221.2 / 102.0 | 221.2 / 128.1 |
20. | Thiophanate methyl | 5.96 | 343.2 / 151.1 | 343.2 / 93.1 |
21. | Propoxur | 5.99 | 210.2 / 168.1 | 210.2 / 111.2 |
22. | Bendiocarb | 6.00 | 224.1 / 109.2 | 224.1 / 167.2 |
23. | Dichlorvos | 6.01 | 220.9 / 109.2 | 220.9 / 95.0 |
24. | Carbofuran | 6.09 | 222.3 / 165.2 | 222.3 / 123.1 |
25. | Pirimicarb | 6.15 | 239.2 / 72.2 | 239.2 / 182.2 |
26. | Carbaryl | 6.32 | 202.3 / 127.1 | 202.3 / 117.2 |
27. | Imazalil | 6.40 | 297.1 / 159.0 | 297.1 / 173.1 |
28. | Isoprocarb | 6.53 | 194.3 / 95.2 | 194.3 / 137.3 |
29. | Metalaxyl | 6.72 | 280.4 / 192.3 | 280.4 / 160.2 |
30. | Metalaxyl-m | 6.72 | 280.4 / 220.3 | 280.4 / 192.1 |
31. | Atrazine | 6.75 | 216.2 / 174.3 | 216.2 / 132.1 |
32. | Atrazine-d5 (IS) | 6.77 | 221.1 / 179.0 | 221.1 / 101.2 |
33. | Isoproturon | 6.86 | 207.2 / 72.3 | 207.2 / 134.3 |
34. | Azinphos-methyl | 6.96 | 318.2 / 160.0 | 318.2 / 132.1 |
35. | Diuron | 6.97 | 233.1 / 72.1 | 233.1 / 160.0 |
36. | Phosmet | 6.97 | 318.1 / 160.2 | 318.1 / 133.0 |
37. | Demeton-O | 6.98 | 259.0 / 89.1 | 259.0 / 61.2 |
38. | Demeton-S | 6.98 | 259.2 / 88.9 | 259.2 / 61.1 |
39. | Nuarimol | 7.08 | 315.0 / 252.1 | 315.0 / 81.0 |
40. | Propanil | 7.11 | 218.2 / 162.0 | 218.2 / 127.0 |
41. | Azoxystrobin | 7.12 | 404.3 / 372.3 | 404.3 / 344.0 |
42. | Malathion | 7.13 | 331.1 / 127.1 | 331.1 / 99.1 |
43. | Methiocarb | 7.14 | 226.1 / 169.1 | 226.1 / 121.1 |
44. | Chlorpropham | 7.20 | 214.1 / 154.0 | 214.1 / 126.1 |
45. | Linuron | 7.20 | 249.2 / 160.1 | 249.2 / 182.1 |
46. | Crotoxyphos | 7.21 | 332.2 / 211.2 | 332.2 / 167.2 |
47. | Promecarb | 7.21 | 208.8 / 109.2 | 208.8 / 151.3 |
48. | Propetamphos | 7.22 | 282.1 / 138.0 | 282.1 / 110.2 |
49. | Boscalid | 7.25 | 343.2 / 307.2 | 343.2 / 140.0 |
50. | Triadimefon | 7.26 | 294.3 / 197.1 | 294.3 / 69.2 |
51. | Triadimenol | 7.35 | 296.3 / 70.2 | 296.3 / 227.1 |
52. | Fenhexamid | 7.40 | 302.1 / 97.1 | 302.1 / 55.0 |
Peaks | tR (min) | MRM 1 | MRM 2 | |
---|---|---|---|---|
53. | Myclobutanil | 7.43 | 289.3 / 70.2 | 289.3 / 124.9 |
54. | Dichlofluanid | 7.44 | 332.9 / 224.0 | 332.9 / 123.1 |
55. | Triazophos | 7.48 | 314.1 / 162.0 | 314.1 / 119.2 |
56. | Alachlor | 7.60 | 270.2 / 238.1 | 270.2 / 162.2 |
57. | Fenarimol | 7.61 | 331.0 / 268.0 | 331.0 / 81.0 |
58. | Iprodione | 7.66 | 330.3 / 245.2 | 332.3 / 247.0 |
59. | Ethoprop | 7.70 | 243.1 / 131.0 | 243.1 / 173.0 |
60. | Parathion | 7.77 | 292.1 / 236.0 | 292.1 / 140.1 |
61. | Fenamiphos | 7.83 | 304.4 / 217.2 | 304.4 / 202.0 |
62. | Diflubenzuron | 7.85 | 311.1 / 158.2 | 311.1 / 141.1 |
63. | Fenoxycarb | 7.87 | 302.1 / 88.0 | 302.1 / 116.1 |
64. | Etaconazole isomer 1 | 7.89 | 328.2 / 159.1 | 328.2 / 123.0 |
65. | Fenbuconazole | 7.89 | 337.3 / 125.3 | 337.3 / 70.3 |
66. | Kresoxim-methyl | 7.90 | 314.2 / 115.9 | 314.2 / 131.0 |
67. | Tolyfluanid | 8.00 | 364.0 / 238.0 | 364.0 / 137.1 |
68. | Etaconazole isomer 2 | 8.01 | 328.3 / 159.2 | 328.3 / 123.1 |
69. | Fenthion | 8.06 | 279.1 / 169.1 | 279.1 / 105.1 |
70. | Quinalphos | 8.07 | 299.3 / 243.1 | 299.3 / 163.2 |
71. | Cyprodinil | 8.16 | 226.1 / 93.3 | 226.1 / 77.1 |
72. | Tebuconazole | 8.24 | 308.3 / 70.1 | 308.3 / 125.1 |
73. | Chlorfenvinphos | 8.32 | 359.2 / 155.1 | 359.2 / 99.2 |
74. | Diazinon | 8.34 | 305.2 / 169.3 | 305.2 / 153.1 |
75. | Pirimiphos methyl | 8.35 | 306.1 / 164.3 | 306.1 / 108.1 |
76. | Phosalone | 8.38 | 368.1 / 182.1 | 368.1 / 138.0 |
77. | Diazinon-d10 (IS) | 8.39 | 315.3 / 170.1 | 315.3 / 154.1 |
78. | Coumaphos | 8.46 | 363.1 / 227.2 | 363.1 / 211.1 |
79. | Propiconazole isomer 1 | 8.60 | 342.3 / 159.0 | 342.3 / 69.3 |
80. | Pyraclostrobin | 8.61 | 388.0 / 164.2 | 388.0 / 194.3 |
81. | Chlorpyrifos methyl | 8.72 | 323.9 / 125.0 | 323.9 / 291.8 |
82. | Propiconazole isomer 2 | 8.77 | 342.4 / 159.1 | 342.4 / 69.4 |
83. | Dialifos | 8.81 | 394.3 / 208.0 | 394.3 / 187.0 |
84. | Prochloraz | 9.01 | 376.1 / 308.1 | 376.1 / 266.0 |
85. | Indoxacarb | 9.04 | 528.6 / 218.0 | 528.6 / 150.2 |
86. | Trifloxystrobin | 9.18 | 409.4 / 186.0 | 409.4 / 145.1 |
87. | Spinosyn A | 9.58 | 733.1 / 142.4 | 733.1 / 98.4 |
88. | Difenoconazole isomer 1 | 9.60 | 406.3 / 251.1 | 408.2 / 253.1 |
89. | Triflumizole | 9.79 | 346.2 / 278.2 | 346.2 / 73.1 |
90. | Difenoconazole isomer 2 | 9.85 | 406.4 / 251.2 | 408.3 / 253.2 |
91. | Ethion | 10.20 | 385.3 / 199.0 | 385.3 / 171.0 |
92. | Spinosyn D | 10.38 | 746.8 / 142.4 | 746.8 / 98.3 |
93. | Chlorpyrifos | 10.40 | 350.0 / 198.0 | 350.0 / 97.0 |
94. | Pendimethalin | 10.47 | 282.3 / 212.2 | 282.3 / 194.3 |
95. | Emamectin B1a benzoate | 10.48 | 887.2 / 158.3 | 887.2 / 126.3 |
96. | Propargite | 10.61 | 368.4 / 175.1 | 368.4 / 231.2 |
97. | Fenpropathrin | 10.67 | 350.3 / 125.0 | 350.3 / 97.4 |
98. | Flufenoxuron | 10.72 | 489.5 / 158.2 | 489.5 / 141.1 |
99. | Lambda cyhalothrin | 10.72 | 467.4 / 225.1 | 467.4 / 181.0 |
100. | Deltamethrin | 10.78 | 523.3 / 280.9 | 523.3 / 181.0 |
101. | trans-Permethrin | 10.90 | 408.4 / 183.3 | 408.4 / 153.2 |
102. | Leptophos | 10.92 | 413.2 / 171.0 | 413.2 / 77.1 |
103. | cis-Permethrin | 10.95 | 408.5 / 183.1 | 408.5 / 153.2 |
104. | Bifenthrin | 10.98 | 440.3 / 181.2 | 440.3 / 166.2 |
Column | Ultra Aqueous C18 (cat.# 9178312) | ||||||||||||||||||||||||||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Dimensions: | 100 mm x 2.1 mm ID | ||||||||||||||||||||||||||||||||||||
Particle Size: | 3 µm | ||||||||||||||||||||||||||||||||||||
Pore Size: | 100 Å | ||||||||||||||||||||||||||||||||||||
Temp.: | 50 °C | ||||||||||||||||||||||||||||||||||||
Standard/Sample | Kale 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 | ||||||||||||||||||||||||||||||||||||
|
Detector | ABSCIEX 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 |
Instrument | API LC-MS/MS |
Sample Preparation | The 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 3000 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 3000 U/min. The sample was diluted 10-fold in mobile phase A before injection. |