LC/MS/MS Analysis of Aflatoxins in Cannabis on Ascentis® Express 2.7 μm Phenyl-Hexyl after Cleanup using Supel™ Tox AflaZea SPE
Materials
analytical column
Ascentis® Express Phenyl-Hexyl, 2.7 μm HPLC Column
2.7 μm particle size, L × I.D. 5 cm × 2.1 mmaccessory
Vials, screw top, silane-treated
volume 2 mL, amber glass vial, O.D. × H × I.D. 12 mm × 32 mm × 4.6 mmstandard
CONDITIONS
sample preparation
Solid Phase Extraction
sample/matrix
cannabis extract spiked with aflatoxins at corresponding concentrations of 6 ppb each (for Aflatoxin B2 and G2) and 24 ppb each (for Afltoxin B1 and G1) in cannabis
SPE tube/cartridge
Supel Tox AflaZea SPE, 6 mL (55314-U)
sample addition
2 mL of sample extract
elution
apply strong vacuum and collect the sample into plastic tube
eluate post-treatment
dilute 0.2 mL of the extract with 0.8 mL distilled water and mix well
column
Ascentis Express Phenyl-Hexyl, 5 cm x 2.1 mm I.D., 2.7 μm particles (53334-U)
mobile phase
[A] 5 mM ammonium formate with 1% formic acid in water; [B] 5 mM ammonium formate with 1% formic acid in methanol
gradient
30% B to 60% B in 3 min; to 100% B in 2 in; held at 100% B for 2 min; to 30% B in 0.1 min; held at 30% B for 1.4 min
flow rate
0.4 mL/min
pressure
5511 psi (380 bar)
column temp.
40 °C
detector
MS, ESI(+), MRM 331.3/189.0, 329.1/243.0, 315.9/259.0, 313.1/241.0
injection
10 μL
Description
Analysis Note
The complex composition of cannabis makes it difficult to apply sample cleanup methods commonly used for other commodities. In this application, interference removal Supel Tox AflaZea SPE was used for sample cleanup providing quick and effective sample preparation prior to mass spectrometric analysis. Sample comprised 0.5 g of finely ground cannabis mixed with 10 mL of 84:16 acetonitrile:water for 30 minutes and centrifuged. It is recommended to use silanized glass vials for this analysis.
Legal Information
Ascentis is a registered trademark of Merck KGaA, Darmstadt, Germany
Supel is a trademark of Sigma-Aldrich Co. LLC