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    气相色谱-质谱法同时测定电子烟油中17种新型吲哚/吲唑酰胺类合成大麻素的含量

    Simultaneous Determination of 17 Novel Indole/Indazole Amide Synthetic Cannabinoids in Electronic Cigarette Oil by Gas Chromatography-Mass Spectrometry

    • 摘要: 电子烟油中可能存在新型吲哚/吲唑酰胺类合成大麻素,为测定其含量并探究其裂解规律,提出了题示方法。取10 μL电子烟油样品(毒品案件缴获)置于15 mL离心管中,用甲醇定容至10.0 mL,涡旋、振荡,静置2 min后,取上清液在HP-5MS毛细管色谱柱上按照柱升温程序分离,质谱分析采用电子轰击(EI)离子源、选择离子监测(SIM)模式,外标法定量。结果显示,17种新型吲哚/吲唑酰胺类合成大麻素的质量浓度在一定范围内与对应的定量离子的峰面积呈线性关系,检出限(3S/N)为1.5~5.0 mg·L−1。对混合标准溶液进行日内(n=6)、日间(n=4)精密度试验和准确度试验,测定值的相对误差和相对标准偏差均小于15%。方法用于实际样品分析,可检出3,3-二甲基-2-1-(4-戊烯-1-基)-1H-吲唑-3-甲酰氨基丁酸甲酯,检出量为31.76 g·L−1

       

      Abstract: There may be novel indole/indazole amide synthetic cannabinoids in electronic cigarette oil. In order to determine their content and explore cracking rules, the title method was proposed. 10 μL of electronic cigarette oil sample (seized in a drug case) was taken and placed in a 15 mL-centrifuge tube, and made its volume up to 10.0 mL with methanol. The mixture was vortexed and shaken, settling for 2 min. The supernatant was separated on a HP-5MS capillary chromatographic column according to the column heating program. Electron impact (EI) ion source and selected ion monitoring (SIM) mode were adopted in mass spectrometry analysis, with external standard method for quantification. As shown by the results, linear relationships between the corresponding quantitative ion response peak areas and mass concentrations of 17 novel indole/indazole amide synthetic cannabinoids were kept in definite ranges, with detection limits (3S/N) in the range of 1.5-5.0 mg·L−1. Intra-day (n=6) and inter-day (n=4) precision tests and accuracy test were carried out on the mixed standard solution, and the relative errors and RSDs of the determined values were less than 15%. The method was applied to the analysis of actual samples, and methyl 3,3-dimethyl-2-1-(pent-4-en-1-yl)-1H-indazole-3-carboxamido butyrate was detected, with the detection amount of 31.76 g·L−1.

       

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