气相色谱-质谱联用法同时测定“电子烟油”中9种吲唑类新型合成大麻素

Simultaneous Determination of 9 Novel Synthetic Indazoles Canna⁃binoids in“E-cigarette Oil”by Gas Chromatography-Mass Spectrometry

针对“电子烟油”中的吲唑类新型合成大麻素物质,建立了气相色谱-质谱联用(GC-MS)分析方法。以地西泮为内标物,待测样本经甲醇提取后,采用HP-5MS色谱柱(30 m×0.25 mm×0.25μm),设置起始温度200℃(保持1 min),以20℃/min升至260℃(保持1 min),再以5℃/min升至300℃(保持10 min)的程序升温条件对9种吲唑类合成大麻素同时进行定性和内标法定量检测,并对目标物的质谱碎片碎裂方式进行解析。结果表明,9种目标物质在20 min内得到有效分离,并在1.0~100.0μg/mL范围内呈良好的线性关系,相关系数(r2)均大于0.997,检出限和定量下限分别为0.04~0.25μg/mL和0.15~0.85μg/mL;加标回收率为95.1%~104%,日内相对标准偏差(RSD)均小于4.6%,日间RSD均小于8.4%。该方法快速、准确,灵敏度高,适用于实际案件检验。

A gas chromatography-mass spectrometric(GC-MS)method was established for the analysis of novel synthetic indazoles cannabinoids in“E-cigarette oil”.The samples were extracted with methanol.With diazepam as internal standard,9 novel synthetic cannabinoids were then determined with an HP-5MS column(30 m×0.25 mm×0.25μm)and quantified by internal standard method under such programmed temperature conditions,namely,setting the initial temperature at 200℃for 1 min,then increasing the temperature to 260℃at a rate of 20℃/min and keeping for 1 min,and finally increasing the temperature to 300℃at a rate of 5℃/min and kept for 10 min.Meanwhile,the mass spectrum of the target fragment fracture manner was analyzed.9 target substances could be effectively separated in 20 min.And the correlation coefficients(r2)were all greater than 0.997 in the linear range of 1.0-100.0μg/mL.The detection limits and quantitation limits were in the ranges of 0.04-0.25μg/mL and 0.15-0.85μg/mL,respectively.The recoveries ranged from 95.1%to 104%,with intra-day relative standard deviations(RSDs)and inter-day RSDs less than 4.6%and 8.4%,respectively.The results showed that the method is effective,accurate and sensitive,and it could be applied to the analysis for actual cases.