GC-MS/MS法测定人头发中的大麻酚类及其代谢物

Analysis of Cannabinoids and The Main Metabolite in Human Hair by GC-MS/MS

目的建立同时检测头发中Δ9-四氢大麻酚(THC)、大麻酚(CBN)、大麻二酚(CBD)和Δ9-四氢大麻酸(THC-COOH)的分析方法。方法头发样品加入氘代内标Δ9-四氢大麻酸(THC-COOH-d3),经碱水解后,以混合溶剂[V(正己烷)∶V(乙酸乙酯=9∶1]进行提取,吹干,残留物经双(三甲基硅烷基)三氟乙酰胺(BSTFA)衍生化,用GC-MS/MS方法进行分析。结果头发中THC-COOH、THC、CBN和CBD的最低检出限分别为4、4、10和20 pg.mg-1,各化合物在0.04～5ng.mg-1呈良好的线性关系(r>0.999),方法精密度、准确度均符合要求。结论本方法选择性强、灵敏度高,适用于头发中CBD、CBN、THC及其代谢物THC-COOH的分析,并成功应用于实际案例中。

Objective To develop a gas chromatography-tandem mass spectrometry （GC-MS/MS） method for the simultaneous analysis of Δ9- tetrahydrocannabinol （THC）, cannabidol （CBD）, cannabinol （CBN） and 11-nor-Δ9-carboxy-tetrahydro- cannabinol （THC-COOH） in human hair. Methods Hair sample was spiked with deuterium labeled 11-nor-Ag-carboxy- te- trahydrocannabinol （THC-COOH-d3） as internal standard, prior to being hydrolyzed with sodium hydroxide. The mixture was extracted with n-hexane/ethyl acetate （9：1）, derived with N, O-his-（trimethylsilyl）-trifluoroacetamide （BSTFA）, and analyzed with GC-MS/MS. Results The limit of detection of THC-COOH, THC, CBN and CBD were 4, 4, 10, and 20pg/mg, respective- ly. Calibration curves covered a range from 0.04 to 5 ng/mg with good linearity （r〉0.999）. The accuracy and precision of analytes all met the requirements. Conclusion The method has a good selectivity and high sensitivity, and is applicable to the analysis of CBD, CBN, THC and their metabolite THC-COOH. It has been verified in real cases.