Skip to Content
MilliporeSigma

LC/MS/MS Analysis of Spice Cannabinoids in Plasma on Ascentis® Express F5 after Solid Phase Extraction (SPE) using HybridSPE®-Phospholipid

LC/MS/MS Analysis of Spice Cannabinoids in Plasma on Ascentis® Express F5 after Solid Phase Extraction (SPE) using HybridSPE®-Phospholipid application for HPLC

Materials

analytical column

Product No.
Description
Pricing

Ascentis® Express F5, 2.7 μm HPLC Column

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

SPE tube or plate

Product No.
Description
Pricing

HybridSPE®-Phospholipid

96-well Plate, bed wt. 50 mg, volume 2 mL, pk of 1

standard

Product No.
Description
Pricing

Spice Cannabinoid Mix solution

100 μg/mL each component in acetonitrile, ampule of 1.0 mL, certified reference material, Cerilliant®

JWH-018 solution

100 μg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®

JWH-073 solution

100 μg/mL in acetonitrile, ampule of 1 mL, certified reference material, Cerilliant®

JWH-073 N-(3-hydroxybutyl) metabolite solution

100 μg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®

CONDITIONS

sample/matrix

rabbit plasma, unfiltered K2-EDTA spiked with Spice cannabinoids (5 ng/mL each)

SPE well plate

HybridSPE-Phospholipid, 96-well plate, 50 mg bed wt., 2 mL well vol (575656-U)

sample addition

to each well add 100 μL plasma, followed by a 300 μL of 1% formic acid in acetonitrile, agitate on orbital shaker for 2 minutes

elution

attach collection plate and apply vacuum at 10” Hg for 4 minutes

column

Ascentis Express F5, 5 cm x 2.1 mm I.D., 2.7 μm particles (53567-U)

mobile phase

[A] 10 mM ammonium formate in water, pH 6.8 (unadjusted); [B] acetonitrile; (50:50; A:B)

flow rate

0.3 mL/min

pressure

1296 psi (89 bar)

column temp.

35 °C

detector

MS, ESI(+), MRM, m/z 344/155 (JWH-073 metabolite), 385/155 (JWH-200), 336/121 (JWH-250), 328/155 (JWH-073), and 342/155 (JWH-018)

injection

2 μL

Description

Analysis Note

Synthetic cannabinoids (Spice) are a relatively new type of designer drug used as a pseudo-legal means to get a cannabis-type high. New synthetic cannabinoids are continually being introduced as suppliers tweak the molecular structures. The ability to rapidly and reliably identify the continually changing population of these compounds in the blood or urine suspected users is a significant analytical challenge facing forensic chemists. A four prong approach using column selectivity, high purity solvents, effective sample prep, and reference standards, was used to develop a method to rapidly isolate and identify Spice cannabinoids from plasma. The Ascentis Express F5 column gave the necessary resolution, and the highest grade LC-MS solvents and additives gave adduct-free response for maximum sensitivity. Sample prep employing the HybridSPE-Phospholipid was rapid and effective and the Cerilliant reference standards enabled confident identification.

Legal Information

Ascentis is a registered trademark of Merck KGaA, Darmstadt, Germany
HybridSPE is a registered trademark of Merck KGaA, Darmstadt, Germany