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Mycotoxins in a CBD Oil Sample on Raptor Biphenyl by LC-MS/MS

LC_GN0587
PeakstR (min)Precursor IonProduct Ion 1Product Ion 2
1.Aflatoxin G2-13C171.340348.3330.3-
2.Aflatoxin G1-13C171.576346.3257.3-
3.Aflatoxin B2-13C171.703332.3303.3-
4.Ochratoxin A1.824404.3239.1358.3
5.Ochratoxin A-13C201.825424.3250.2-
6.Aflatoxin B1-13C171.947330.3301.4-
ColumnRaptor Biphenyl (cat.# 9309A52)
Dimensions:50 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.:35 °C
Sample
Diluent:45:55 Water:Methanol
Inj. Vol.:5 µL
Mobile Phase
A:Water, 2 mM ammonium formate, 0.1% formic acid
B:Methanol, 2 mM ammonium formate, 0.1% formic acid
Time (min)Flow (mL/min)%A%B
0.000.73565
2.000.71090
2.010.73565
3.000.73565
DetectorMS/MS
Ion Mode:ESI+
Mode:MRM
InstrumentUHPLC
Notes0.25 g of commercially available hemp-derived CBD oil was weighed into a 2 mL vial. A working internal standard was prepared using 13C labeled analogs at a concentration of 250 ng/mL in methanol. 10 µL of the working internal standard was aliquoted into the sample followed by vortexing for 10 seconds at 3,000 rpm. 1 mL of 45:55 H2O:MeOH was added to the sample. The sample was vortexed for 30 seconds at 3,000 rpm. The sample was then centrifuged at 3,000 xg for 5 min at 10 °C. 750 µL of the supernatant was transferred to a conditioned (1 mL 45:55 water:methanol) Resprep bonded reversed phase SPE cartridge (Restek cat.# 26030). The sample was pulled through under vacuum into an autosampler vial for LC-MS/MS analysis.