LC/MS/MS Analysis of Spice Cannabinoids in Plasma on Ascentis® Express F5 after Solid Phase Extraction (SPE) using HybridSPE®-Phospholipid
材料
SPE 管或板
分析色谱柱
标准
5种大麻素混标 溶液
100 μg/mL each component in acetonitrile, ampule of 1.0 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
说明
分析说明
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.
法律信息
Ascentis is a registered trademark of Merck KGaA, Darmstadt, Germany
HybridSPE is a registered trademark of Merck KGaA, Darmstadt, Germany