GC Analysis of Pesticide Residues in Cannabis on SLB®-5ms after QuEChERS Extraction then QuEChERS Cleanup using Supel™ QuE Verde

GC Analysis of Pesticide Residues in Cannabis on SLB®-5ms after QuEChERS Extraction then QuEChERS Cleanup using Supel™ QuE Verde

Conditions

sample preparation Solid Phase Extraction (QuEChERS, Dispersive)
sample preparation place supernatant in amber low adsorption vial for GC/MS/MS analysis.
sample/matrix ground cannabis, 1 gm
extraction tube Supel QuE Citrate (55227-U)
extraction process Add 10 mL water to sample, allow to sit for 30 min. Add 10 mL of acetontrile containing 1% acetic acid; shake 10 min at 2500 rpm on automated shaker. (add contents of Supel QuE citrate extraction tube; shake 1 min; centrifuge at 5000 rpm for 5 min; remove supernatant)
clean-up process transfer 1 mL of supernatant to Supel QuE Verde cleanup tube; (shake for 2 min; centrifuge at 5000 rpm for 5 min; remove supernatant)
clean-up tube Supel QuE Verde, 2 mL cleanup tube (55447-U)
column SLB-5ms, 30 m x 0.25 mm I.D. x 0.25 µm (28471-U)
oven 50 °C (2 min), 8 °C/min to 320 °C (5 min)
carrier gas helium, 1.4 mL/min, constant
injection 1 µL, splitless (splitter open at 0.75 min)
liner 4 mm I.D. FocusLiner inlet liner (with taper)
inj. temp. 250 °C
detector MS/MS
MSD interface 320 °C
scan range MRM

Description

Analysis Note There are no official test methods for the determination of pesticide residues in cannabis. However a potential approach is the use of the “quick, easy, cheap, effective, rugged and safe” (QuEChERS) method outlined in AOAC official method 2007.01. In this application, QuEChERS was used in the extraction of pesticides from dried cannabis followed by cleanup using Supel QuE Verde sorbent blend. This blend consists of (primary-secondary amine) PSA, Z-Sep+ and an improved Graphitized Carbon Black (GCB), which provides better recoveries of planar pesticides than traditional GCBs. When used to clean samples containing chlorophyll, Supel QuE Verde will provide better recovery of planar pesticides than blends containing traditional GCB.
In this application, cannabis obtained courtesy of Dr. Hari H. Singh, Program Director at the Chemistry & Physiological Systems Research Branch of the National Institute on Drug Abuse at the National Institute of Health was spiked at 50 ng/g with pesticides of interest in cannabis testing. After QuEChERS extraction, replicate samples were cleaned using Supel QuE Verde and analyzed by GC/MS/MS for determination of recovery and reproducibility.
Categories Analytical Chromatography, GC Applications, Pesticides
Featured Industry Agriculture
Legal Information Supel is a trademark of Sigma-Aldrich Co. LLC, SLB is a registered trademark of Sigma-Aldrich Co. LLC
suitability application for GC, application for SPE

Materials

     
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