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G1007613

LC/MS/MS Analysis of Pesticides in Cannabis on the Ascentis® RP-Amide after QuEChERS Extraction and Cleanup Using Supel™ QuE Verde

application for LC-MS, application for SPE

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technique(s)

LC/MS: suitable
solid phase extraction (SPE): suitable

test parameters

sample preparation: Dispersive (QuEChERS)
sample/matrix: 1.9 g of cannabis spiked with pesticides at 50 ng/g
extraction tube: Supel QuE Citrate extraction tube (55227-U)
extraction process: add 10 mL of acetonitrile; shake for 30 minutes at 2500 rpm on shaker; add contents of Supel QuE citrate extraction tube; (shake immediately for 1 minute; centrifuge at 5000 rpm for 5 minutes)
clean-up tube: Supel QuE Verde, 2 mL (55227-U)
clean-up process: transfer 1 mL of acetonitrile layer into Supel QuE Verde cleanup tube; shake for 1 minutes; (centrifuge at 5000 rpm for 3 minutes; draw of supernatant for LC/MS/MS analysis)
column: Ascentis RP-Amide, 10 cm x 2.1 mm I.D., 3.0 μm particles (565301-U)
column: Ascentis RP-Amide Supelguard guard cartridge, 2 cm x 2.1 mm I.D., 5 μm particles (565372-U)
mobile phase: [A] 5 mM ammonium formate, 0.1% formic acid in 95:5 water:acetonitrile; [B] 5 mM ammonium formate, 0.1% formic acid in 5:95 water:acetonitrile
gradient: 10% B held for 1 min; to 100% B in 13 min; held at 100% B for 6 min; to 10% in 0.5 min; held at 10% B for 6 min
flow rate: 0.4 mL/min
column temp.: 30 °C
detector: MRM
injection: 5 μL
sample: QuEChERS extract of cannabis in acetonitrile

suitability

application for LC-MS
application for SPE

application(s)

environmental

Analysis Note

Consumption of cannabis and/or cannabis based products is currently legal in some form in 28 US states plus the District of Columbia. Pesticide testing on plant material and extracts is required in some states, including Oregon, which mandates a specific target list for testing. A common approach used by testing labs for pesticides is QuEChERS extraction followed by a dispersive cleanup. In this application a majority of the LC-amenable pesticides on the Oregon list were extracted from cannabis spiked at 50 ng/g using QuEChERS, followed by cleanup with Supel™ QuE Verde. Analysis was achieved using the Ascentis® RP-Amide column equipped with a guard. Supel QuE Verde offered sufficient background reduction for LC/MS/MS analysis with recoveries of 70-120% for a majority of the pesticides.

Other Notes

Sample pretreatment: Added 10 mL of deionized water, mixed and equilibrated for 10 minutes

Legal Information

Ascentis is a registered trademark of Merck KGaA, Darmstadt, Germany
Supel is a trademark of Sigma-Aldrich Co. LLC

Analyte

Description
    Daminozide
    Acephate
    Oxamyl
    Methomyl
    Thiamethoxam
    Flonicamid
    Imidacloprid
    Dimethoate
    Acetamiprid
    Aldicarb
    Thiacloprid
    Imazalil (Enilconazole)
    Dichlorvos
    Propoxur
    Spiroxamine
    Carbofuran
    Metalaxyl
    Carbaryl
    Spinosyn A
    Spinosyn D
    Spirotetramat
    Paclobutrazol
    Chlorantraniliprole
    Methiocarb (Mercaptodimethur)
    Myclobutanil
    Azoxystrobin
    Ethoprop (Ethoprophos)
    Phosmet (Imidan)
    Tebuconazole
    Boscalid (Nicobifen)
    Bifenazate (D 2341)
    Malathion
    Propiconazole
    Fenoxycarb
    Kresoxim methyl
    Clofentezin
    Prallethrin
    Trifloxystrobin
    Piperonyl butoxide
    Fenpyroximate (E)
    Hexylthiazox
    Etoxazole
    Spiromesifen
    Pyrethrin
    Pyridaben
    See All (45)

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