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California Cannabis Pesticides and Mycotoxins in Gummy Edibles on Raptor ARC-18
| Peaks | tR (min) | Precursor Ion | Product Ion 1 | Product Ion 2 | Polarity | |
|---|---|---|---|---|---|---|
| 1. | Daminozide-d6 | 0.7 | 167.0 | 149.3 | 49.3 | + |
| 2. | Daminozide | 0.7 | 161.1 | 44.1 | 143.2 | + |
| 3. | Acephate | 1.7 | 184.0 | 143.1 | 95.1 | + |
| 4. | Oxamyl | 2.0 | 237.1 | 72.1 | 90.1 | + |
| 5. | Flonicamid | 2.1 | 230.1 | 203.1 | 174.1 | + |
| 6. | Methomyl | 2.1 | 163.1 | 88.1 | 106.1 | + |
| 7. | Thiamethoxam | 2.1 | 292.0 | 211.1 | 181.1 | + |
| 8. | Imidacloprid | 2.3 | 256.1 | 209.1 | 175.1 | + |
| 9. | Mevinphos | 2.4 | 225.1 | 127.1 | 193.2 | + |
| 10. | Acetamiprid | 2.4 | 223.0 | 126.1 | 56.1 | + |
| 11. | Dimethoathe-d6 | 2.4 | 236.1 | 205.1 | - | + |
| 12. | Dimethoate | 2.4 | 230.0 | 199.1 | 125.1 | + |
| 13. | Thiacloprid | 2.5 | 253.0 | 126.0 | 90.1 | + |
| 14. | Aflatoxin G2 | 2.5 | 331.2 | 189.3 | 115.2 | + |
| 15. | Aflatoxin G1 | 2.5 | 329.2 | 243.2 | 215.3 | + |
| 16. | Aldicarb | 2.6 | 116.0 | 89.2 | 70.2 | + |
| 17. | Aflatoxin B2 | 2.6 | 315.3 | 287.2 | 243.3 | + |
| 18. | Dichlorvos | 2.7 | 220.9 | 109.1 | 79.2 | + |
| 19. | Dichlorvos-d6 | 2.7 | 227.0 | 115.1 | - | + |
| 20. | Aflatoxin B1 | 2.7 | 313.2 | 241.2 | 128.2 | + |
| 21. | Imazalil | 2.7 | 297.0 | 159.0 | 201.0 | + |
| 22. | Carbofuran | 2.7 | 222.1 | 123.1 | 165.2 | + |
| 23. | Propoxur | 2.7 | 210.1 | 111.1 | 93.1 | + |
| 24. | Carbaryl-d7 | 2.8 | 209.2 | 152.2 | - | + |
| 25. | Carbaryl | 2.8 | 202.1 | 145.1 | 127.1 | + |
| 26. | Diuron-d6 | 3.0 | 239.1 | 78.2 | - | + |
| 27. | Atrazine-d5 | 3.0 | 221.2 | 179.1 | - | + |
| 28. | Naled | 3.1 | 397.8 | 127.1 | 109.1 | + |
| 29. | Metalaxyl | 3.1 | 280.2 | 220.2 | 192.2 | + |
| 30. | Spiroxamine | 3.1 | 298.3 | 144.2 | 100.2 | + |
| 31. | Chlorantraniliprole | 3.2 | 483.9 | 452.9 | 285.9 | + |
| 32. | Phosmet | 3.2 | 318.0 | 160.1 | 77.2 | + |
| 33. | Azoxystrobin | 3.3 | 404.0 | 372.1 | 344.1 | + |
| 34. | Linuron-d6 | 3.3 | 255.1 | 160.1 | - | + |
| 35. | Fludioxonil | 3.4 | 247.0 | 180.0 | 126.0 | - |
| 36. | Methiocarb | 3.4 | 226.1 | 169.1 | 121.1 | + |
| 37. | Dimethomorph | 3.5 | 388.2 | 301.2 | 165.3 | + |
| 38. | Boscalid | 3.5 | 342.9 | 307.1 | 140.1 | + |
| 39. | Paclobutrazol | 3.6 | 294.3 | 70.1 | 125.1 | + |
| 40. | Malathion | 3.6 | 331.0 | 127.2 | 285.2 | + |
| 41. | Myclobutanil | 3.7 | 289.1 | 70.1 | 125.1 | + |
| 42. | Bifenazate | 3.7 | 301.0 | 198.1 | 170.2 | + |
| 43. | Ochratoxin A | 3.8 | 404.2 | 239.1 | 358.3 | + |
| 44. | Fenhexamid | 3.9 | 302.1 | 97.1 | 55.2 | + |
| 45. | Spirotetramat | 4.0 | 374.2 | 302.1 | 216.1 | + |
| 46. | Ethoprophos | 4.1 | 243.1 | 131.1 | 97.1 | + |
| 47. | Fipronil | 4.1 | 436.8 | 331.8 | 251.9 | - |
| 48. | Fenoxycarb | 4.2 | 302.1 | 88.1 | 116.1 | + |
| 49. | Kresoxim-methyl | 4.4 | 314.2 | 267.2 | 222.2 | + |
| 50. | Tebuconazole | 4.4 | 308.1 | 70.1 | 125.1 | + |
| 51. | Diazinon-d10 | 4.6 | 315.2 | 170.2 | - | + |
| 52. | Spinosyn A (Spinosad) | 4.6 | 732.4 | 142.2 | 98.1 | + |
| 53. | Diazinon | 4.6 | 305.1 | 169.2 | 153.2 | + |
| 54. | Coumaphos | 4.7 | 363.1 | 227.1 | 307.1 | + |
| 55. | Pyridaben | 4.7 | 365.1 | 309.2 | 147.2 | + |
| 56. | Propiconazole | 4.7 | 342.0 | 159.0 | 69.2 | + |
| 57. | Clofentezine | 4.8 | 303.0 | 138.1 | 102.1 | + |
| 58. | Spinosyn D (Spinosad) | 5.0 | 746.5 | 142.3 | 98.4 | + |
| 59. | Spinosyn J (Spinetoram) | 5.1 | 748.5 | 142.3 | 98.3 | + |
| 60. | Trifloxystrobin | 5.3 | 409.2 | 186.1 | 145.1 | + |
| 61. | Prallethrin | 5.3 | 301.2 | 123.2 | 105.2 | + |
| 62. | Pyrethrin II | 5.5 | 373.1 | 161.1 | 133.2 | + |
| 63. | Spinosyn L (Spinetoram) | 5.6 | 760.5 | 142.2 | 98.1 | + |
| 64. | Piperonyl butoxide | 6.0 | 356.3 | 177.2 | 119.2 | + |
| 65. | Chlorpyrifos | 6.1 | 349.9 | 198.0 | 97.1 | + |
| 66. | Hexythiazox | 6.2 | 353.1 | 228.1 | 168.1 | + |
| 67. | Etoxazole | 6.6 | 360.2 | 141.1 | 304.2 | + |
| 68. | Spiromesifen | 6.7 | 273.2 | 255.2 | 187.2 | + |
| 69. | Pyrethrin I | 6.9 | 329.2 | 161.2 | 105.2 | + |
| 70. | Cyfluthrin (qualifier) | 6.9 | 453.1 | 193.2 | - | + |
| 71. | Cyfluthrin | 6.9 | 451.1 | 191.2 | - | + |
| 72. | Cypermethrin | 7.1 | 433.1 | 191.0 | 416.0 | + |
| 73. | Fenpyroximate | 7.1 | 422.2 | 366.1 | 138.1 | + |
| 74. | trans-Permethrin | 7.6 | 408.3 | 183.2 | 355.1 | + |
| 75. | cis-Permethrin | 7.9 | 408.3 | 183.2 | 355.1 | + |
| 76. | Avermectin B1a | 7.9 | 890.5 | 305.4 | 567.4 | + |
| 77. | Etofenprox | 8.0 | 394.3 | 177.2 | 359.3 | + |
| 78. | Bifenthrin | 8.2 | 440.0 | 181.2 | 166.2 | + |
| 79. | Acequinocyl (precursor ion 1) | 9.4 | 402.3 | 343.2 | 189.0 | + |
| 80. | Acequinocyl (precursor ion 2) | 9.4 | 386.0 | 344.2 | 189.1 | + |
LC_GN0666
| Column | Raptor ARC-18 (cat.# 9314A12) | ||||||||||||||||||||||||||||||||
| Dimensions: | 100 mm x 2.1 mm ID | ||||||||||||||||||||||||||||||||
| Particle Size: | 2.7 µm | ||||||||||||||||||||||||||||||||
| Pore Size: | 90 Å | ||||||||||||||||||||||||||||||||
| Guard Column: | Raptor ARC-18 EXP guard column cartridge 5 mm, 2.1 mm ID, 2.7 µm (cat.# 9314A0252) | ||||||||||||||||||||||||||||||||
| Temp.: | 40 °C | ||||||||||||||||||||||||||||||||
| Sample | California pesticide standard #1 (cat.# 34124) | ||||||||||||||||||||||||||||||||
| California pesticide standard #2 (cat.# 34125) | |||||||||||||||||||||||||||||||||
| California pesticide standard #3 (cat.# 34126) | |||||||||||||||||||||||||||||||||
| California pesticide standard #4 (cat.# 34127) | |||||||||||||||||||||||||||||||||
| California pesticide standard #5 (cat.# 34128) | |||||||||||||||||||||||||||||||||
| California pesticide standard #6 (cat.# 34129) | |||||||||||||||||||||||||||||||||
| Dimethoate-d6 (cat.# 31988) | |||||||||||||||||||||||||||||||||
| Dichlorvos-d6 (cat.# 31987) | |||||||||||||||||||||||||||||||||
| Carbaryl-d7 (cat.# 31985) | |||||||||||||||||||||||||||||||||
| Diazinon-d10 (cat.# 31986) | |||||||||||||||||||||||||||||||||
| Atrazine-d5 (cat.# 31984) | |||||||||||||||||||||||||||||||||
| Diuron-d6 (cat.# 31989) | |||||||||||||||||||||||||||||||||
| Liuron-d6 (cat.# 31990) | |||||||||||||||||||||||||||||||||
| Aflatoxins standard (cat.# 34121) | |||||||||||||||||||||||||||||||||
| Ochratoxin A (cat.# 34122) | |||||||||||||||||||||||||||||||||
| Compounds not present in these mixes were obtained separately. | |||||||||||||||||||||||||||||||||
| Diluent: | 75:25 Acetonitrile:water | ||||||||||||||||||||||||||||||||
| Conc.: | 3.75-15 ng/mL (Expected concentration range in extract of gummy initially spiked at 100 ng/g.) | ||||||||||||||||||||||||||||||||
| Inj. Vol.: | 2 µL | ||||||||||||||||||||||||||||||||
| Mobile Phase | |||||||||||||||||||||||||||||||||
| A: | Water, 2 mM ammonium formate, 0.1% formic acid | ||||||||||||||||||||||||||||||||
| B: | Methanol, 2 mM ammonium formate, 0.1% formic acid | ||||||||||||||||||||||||||||||||
| |||||||||||||||||||||||||||||||||
| Detector | MS/MS | ||||||||||||||||||||||||||||||||
| Ion Mode: | ESI+/ESI- | ||||||||||||||||||||||||||||||||
| Mode: | MRM | ||||||||||||||||||||||||||||||||
| Instrument | UHPLC | ||||||||||||||||||||||||||||||||
| Notes | Gummies were manually chopped into small pieces, and 1 g of sample was weighed in a 50 mL polypropylene tube. The sample was mixed with 5 mL of water and then vigorously vortexed until all gummy pieces were fully solubilized. The sample was fortified with pesticides and mycotoxins at 100 ng/g. A mix of internal standards was added at 200 ng/g. The spiked sample was further vortexed for 30 sec. 5 mL of acetonitrile acidified with 1% acetic acid was added to the sample, and this was followed by a 30 sec vortex agitation. Then, a pouch of European EN 15662 QuEChERS extraction salts (cat.# 25849) was added to the sample. The sample was vortexed for 30 sec and then centrifuged for 5 min. 750 µL of organic extract was mixed with 250 µL of water. 2 μL of final extract was injected into the LC-MS/MS system. |
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