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Peaks | tR (min) | Precursor Ion | Product Ion 1 | Product Ion 2 | |
---|---|---|---|---|---|
1. | Nivalenol | 0.92 | 295.1 | 137.1 | 91.0 |
2. | Patulin | 1.03 | 155.0 | 99.0 | 81.0 |
3. | Ergometrine | 1.27 | 326.2 | 223.2 | 208.1 |
4. | Deoxynivalenol | 1.30 | 297.2 | 231.0 | 249.0 |
5. | Ergometrinine | 1.83 | 326.2 | 223.2 | 208.1 |
6. | Fusarenon-X | 1.98 | 355.1 | 137.1 | 247.1 |
7. | 15-Acetyldeoxynivalenol | 3.14 | 339.2 | 137.1 | 321.2 |
8. | 3-Acetyldeoxynivalenol | 3.21 | 339.2 | 213.1 | 231.1 |
9. | Tenuazonic acid | 4.22 | 198.1 | 125.0 | 153.1 |
10. | Altenuene | 4.70 | 293.2 | 257.1 | 275.2 |
11. | Alternariol | 5.30 | 259.0 | 185.1 | 130.0 |
12. | Citrinin | 5.43 | 251.2 | 233.1 | 205.1 |
13. | Ergosine | 5.47 | 548.4 | 208.1 | 223.2 |
14. | Fumonisin B1 | 5.63 | 722.5 | 352.3 | 334.2 |
15. | Ergosinine | 5.67 | 548.4 | 208.1 | 223.2 |
16. | Diacetoxyscirpenol | 5.73 | 384.2 | 247.1 | 307.2 |
17. | Ergotamine | 5.90 | 582.4 | 223.2 | 268.2 |
18. | Ergocornine | 6.03 | 562.4 | 268.2 | 223.2 |
Peaks | tR (min) | Precursor Ion | Product Ion 1 | Product Ion 2 | |
---|---|---|---|---|---|
19. | Ergotaminine | 6.13 | 582.4 | 223.2 | 268.2 |
20. | HT-2 | 6.20 | 447.2 | 345.1 | 285.1 |
21. | Fumonisin B3 | 6.32 | 706.4 | 336.2 | 318.3 |
22. | Ergocryptine | 6.32 | 576.4 | 268.2 | 223.2 |
23. | Ergocristine | 6.56 | 610.4 | 223.2 | 592.4 |
24. | Fumonisin B2 | 6.68 | 706.4 | 336.2 | 318.3 |
25. | Tentoxin | 6.70 | 415.2 | 312.2 | 302.2 |
26. | α-Zearalenol | 6.96 | 303.1 | 285.1 | 175.0 |
27. | Ergocorninine | 7.07 | 562.4 | 268.2 | 223.2 |
28. | T-2 | 7.14 | 489.2 | 387.1 | 245.1 |
29. | Aflatoxin G2 | 7.15 | 331.2 | 189.0 | 313.0 |
30. | Ergocryptinine | 7.31 | 576.4 | 268.2 | 223.2 |
31. | Ergocristinine | 7.53 | 610.4 | 223.2 | 592.4 |
32. | Aflatoxin G1 | 7.62 | 329.1 | 199.7 | 243.0 |
33. | Zearalenone | 7.65 | 319.2 | 283.1 | 187.0 |
34. | Alternariol monomethylether | 7.69 | 273.0 | 199.1 | 128.0 |
35. | Aflatoxin B2 | 7.81 | 315.1 | 287.0 | 259.0 |
36. | Aflatoxin B1 | 8.20 | 313.2 | 241.1 | 284.9 |
37. | Ochratoxin A | 8.31 | 404.1 | 239.0 | 358.0 |
Column | Raptor Biphenyl (cat.# 9309A12) | ||||||||||||||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Dimensions: | 100 mm x 2.1 mm ID | ||||||||||||||||||||||||
Particle Size: | 2.7 µm | ||||||||||||||||||||||||
Pore Size: | 90 Å | ||||||||||||||||||||||||
Guard Column: | Raptor Biphenyl EXP guard column cartridge 5 mm, 2.1 mm ID, 2.7 µm (cat.# 9309A0252) | ||||||||||||||||||||||||
Temp.: | 60 °C | ||||||||||||||||||||||||
Standard/Sample | Aflatoxins standard (cat.# 34121) | ||||||||||||||||||||||||
Ochratoxin A standard (cat.# 34122) | |||||||||||||||||||||||||
Diluent: | 50:50 Water:methanol | ||||||||||||||||||||||||
Conc.: | 6.25 ng/mL final concentration after sample preparation | ||||||||||||||||||||||||
Inj. Vol.: | 5 µL | ||||||||||||||||||||||||
Mobile Phase | |||||||||||||||||||||||||
A: | Water, 0.05% formic acid | ||||||||||||||||||||||||
B: | Methanol, 0.05% formic acid | ||||||||||||||||||||||||
|
Detector | MS/MS |
---|---|
Ion Mode: | ESI+ |
Mode: | MRM |
Instrument | UHPLC |
Sample Preparation | A blended flour was prepared by mixing white rice flour (75%); brown rice flour (5%); millet flour (5%); oat flour (5%); all-purpose wheat flour (5%); and all-purpose, gluten-free flour (5%). Two grams of the flour sample were weighed into a 50-mL polypropylene centrifuge tube (cat.# 25846) and fortified at 50 µg/kg for all analytes with a stock standard solution. After sitting at room temperature for 10 minutes, 16 mL of extraction solution (80:20 acetonitrile:water) containing 0.5% formic acid were added, and the tube was stirred to create a homogenous suspension. The extraction was carried out by shaking horizontally on a digital pulse mixer (Glas-Col LLC, Terre Haute, IN) at 800 rpm for 20 minutes. After centrifuging for 5 minutes at 4000 rpm, 1 mL of extract was evaporated to dryness at 45 °C under a gentle stream of nitrogen. The dried extract was reconstituted with 1 mL of 50:50 water:methanol solution, and a 0.4 mL aliquot was transferred to and filtered using a Thomson SINGLE StEP filter vial with a 0.2 µm PTFE filter (cat.# 25874). Five µL of the filtered solution was injected for the LC-MS/MS analysis. |
Notes | The chromatogram shows peaks with the MS transition of product ion 1. Note that method development work demonstrated that whenever a new column is installed it must be rinsed and maintained under mobile phase overnight to ensure an acceptable peak shape for tenuazonic acid. |