Merck

LC/MS/MS Analysis of Aflatoxins in Cannabis on Ascentis® Express 2.7 μm Phenyl-Hexyl after Cleanup using Supel Tox AflaZea SPE

LC/MS/MS Analysis of Aflatoxins in Cannabis on Ascentis® Express 2.7 μm Phenyl-Hexyl after Cleanup using Supel™ Tox AflaZea SPE application for LC-MS, application for SPE

Materials

analytical column

Product No.
Description
Pricing

Ascentis® Express Phenyl-Hexyl, 2.7 μm HPLC Column

2.7 μm particle size, L × I.D. 5 cm × 2.1 mm

accessory

Product No.
Description
Pricing

Black plastic caps

Solid top, white rubber liner, thread for 8-425, pkg of 1000 ea

Visiprep SPE Vacuum Manifold

DL (Disposable Liner), 12-port model

Disposable Liners for Visiprep DL Manifolds (included with 57044 and 57265)

PTFE, pk of 100

Vials, screw top, silane-treated

volume 2 mL, amber glass vial, O.D. × H × I.D. 12 mm × 32 mm × 4.6 mm

QuEChERS Shaker and Rack Starter Kit

AC/DC input 115 V AC (USA Compatible Plug)

standard

Product No.
Description
Pricing

Aflatoxin Mix 4 solution

analytical standard

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