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Ergot Alkaloid Epimers in Fortified Flour Sample on Raptor Biphenyl by LC-MS/MS

LC_FS0551
PeakstR (min)Precursor IonProduct Ion 1Product Ion 2
1.Ergometrine1.27326.2223.2208.1
2.Ergometrinine1.83326.2223.2208.1
3.Ergosine5.47548.4208.1223.2
4.Ergosinine5.67548.4208.1223.2
5.Ergotamine5.90582.4223.2268.2
6.Ergocornine6.03562.4268.2223.2
PeakstR (min)Precursor IonProduct Ion 1Product Ion 2
7.Ergotaminine6.13582.4223.2268.2
8.Ergocryptine6.32576.4268.2223.2
9.Ergocristine6.56610.4223.2592.4
10.Ergocorninine7.07562.4268.2223.2
11.Ergocryptinine7.31576.4268.2223.2
12.Ergocristinine7.53610.4223.2592.4
ColumnRaptor 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
Time (min)Flow (mL/min)%A%B
0.000.47525
5.000.45050
9.000.40100
9.010.47525
11.00.47525
DetectorMS/MS
Ion Mode:ESI+
Mode:MRM
InstrumentUHPLC
Sample PreparationA 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.