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Peaks | tR (min) | Precursor Ion | Product Ion 1 | Product Ion 2 | |
---|---|---|---|---|---|
1. | Ergometrine | 1.27 | 326.2 | 223.2 | 208.1 |
2. | Ergometrinine | 1.83 | 326.2 | 223.2 | 208.1 |
3. | Ergosine | 5.47 | 548.4 | 208.1 | 223.2 |
4. | Ergosinine | 5.67 | 548.4 | 208.1 | 223.2 |
5. | Ergotamine | 5.90 | 582.4 | 223.2 | 268.2 |
6. | Ergocornine | 6.03 | 562.4 | 268.2 | 223.2 |
Peaks | tR (min) | Precursor Ion | Product Ion 1 | Product Ion 2 | |
---|---|---|---|---|---|
7. | Ergotaminine | 6.13 | 582.4 | 223.2 | 268.2 |
8. | Ergocryptine | 6.32 | 576.4 | 268.2 | 223.2 |
9. | Ergocristine | 6.56 | 610.4 | 223.2 | 592.4 |
10. | Ergocorninine | 7.07 | 562.4 | 268.2 | 223.2 |
11. | Ergocryptinine | 7.31 | 576.4 | 268.2 | 223.2 |
12. | Ergocristinine | 7.53 | 610.4 | 223.2 | 592.4 |
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 | |||||||||||||||||||||||||
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. |
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