Detection of Synthetic Cannabinoid CUMYL-PEGACLONE in E-Cigarette Oil and Hair / 法医学杂志

OBJECTIVES@#To establish a combined high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) and gas chromatography-mass spectrometry (GC-MS) method to detect the synthetic cannabinoid CUMYL-PEGACLONE in e-cigarette oil and hair.@*METHODS@#HPLC-MS/MS and GC-MS were used to establish the detection method of CUMYL-PEGACLONE, and the hair of drug-involved persons and the seized e-cigarette oil were detected.@*RESULTS@#The main mass spectrometry characteristic ions m/z of CUMYL-PEGACLONE measured by GC-MS were 91, 179, 197, 254 and 372. CUMYL-PEGACLONE had a good linear relationship in the mass concentration range of 2-50 ng/mL, and the linear correlation coefficient (r) was greater than 0.99. The limit of detection (LOD) of CUMYL-PEGACLONE in hair was 0.01 ng/mg, and the limit of quantitation (LOQ) was 0.02 ng/mg. The LOD of CUMYL-PEGACLONE in e-cigarette oil was 1 ng/mg, and the LOQ was 2 ng/mg. The average recoveries of CUMYL-PEGACLONE under the attempt at high, intermediate and low levels in blank human hair and e-cigarette oil matrix were 98.2%-132.4% and 93.5%-110.6%, and the intraday and intraday precision were 1.2%-12.9% and 0.7%-2.9%. CUMYL-PEGACLONE was detected in the hair of 15 drug-involved persons. Except for 1 person who was lower than LOQ, the concentration of CUMYL-PEGACLONE in the hair of other 14 persons was 0.035-0.563 ng/mg. The mass fraction of CUMYL-PEGACLONE in 2 e-cigarette oil were 0.17% and 0.21%, respectively.@*CONCLUSIONS@#The established HPLC-MS/MS and GC-MS methods are applied to the detection of HPLC-MS/MS in drug-related cases, which provides strong evidence support for the handling authority to quickly investigate these cases, and also provides a reference for the identification of such substances in future.

Determination of Low-concentration Clenbuterol in Edible Meat Using High Performance Liquid Chromatography-tandem Mass Spectrometry / 中国运动医学杂志

Objective To determine low-concentration clenbuterol in edible meat based on the solidphase extraction coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).Method The homogenated sample was acidized to remove proteins,and purified using the liquid-liquid extraction and MCX Oasis solid prepared extraction column,then further treated with gradient elution with the mobile phase of ammonium formate (10 mmol/L and pH 3.5) and acetonitrile.The clenbuterol was completely separated on Eclipse C18 (1.8 μm,4.6×100 mm) column and detected in multiple reaction monitoring (MRM) mode.Results A good linearity was achieved for clenbuterol in the arrange of 0.01～0.2 μg/kg based on the internal standard calibration of D9-clenbuterol,with the linearity correlation coefficient greater than 0.99 and the detection limit of 0.005 μg/kg.The relative recovery of target compounds spiked in blank sample at three levels ranging from 78.8 to 114.8％,with the relative standard deviations less than 10％.Conclusion The method in this research is simple,rapid,reliable and suitable to confirm low-concentration clenbuterol in edible meat.