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微分段分析多根头发中20种苯二氮?类药物及案例应用

Micro-segmention analysis of 20 benzodiazepines in multiple hairs and case application

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【作者】 谢琳溪; 薛鼎昌; 郭兆辰; 任飞; 李婧; 贠克明; 尉志文; 张潮; 辛国斌;

【Author】 Xie Linxi;Xue Dingchang;Guo Zhaochen;Ren Fei;Li Jing;Yun Keming;Wei Zhiwen;Zhang Chao;Xin Guobin;Shanxi Medical University;Taiyuan Public Security Bureau;Inner Mongolia University of Science and Technology;Beijing Municipal Public Security Bureau;

【通讯作者】 任飞;贠克明;尉志文;

【机构】 山西医科大学; 太原市公安局; 内蒙古科技大学; 北京市公安局;

【摘要】 目的 建立一种基于多根头发微分段分析的LC-MS/MS的分析方法,并对20种苯二氮?类药物在1 mm头发中的检测进行验证,并最终用于案件检测分析。方法 将5根头发每根切成1mm长的片段,并将相应段落放在一起,在含二硫苏糖醇、甲醇等的提取液中浸泡并进行超声处理。流动相A为0.1%甲酸水,流动相B为乙腈。采用电喷雾离子源正离子模式,在多反应监测模式下采集数据。结果 多根头发中20种苯二氮?类药物在各自线性范围内线性关系良好(r> 0.99),检出限为0.2~5 pg/mm,最低定量限为0.5~20 pg/mm,日内、日间精密度为2.03%~13.81%,日内、日间准确度为87.98%~111.29%,基质效应为71.15%~110.43%,提取回收率为69.34%~99.94%。用该方法对单次服用氯硝西泮20 d的志愿者进行头发样本分析,15根头发中氯硝西泮检出位置距发根第6~11段,浓度范围为1.06~3.45 pg/mm。并用此方法对案件中疑似被服用过安眠药受害者毛发进行分析,15根头发中在距发根第9~13段检出氯硝西泮成分,定量结果 1.07~19.06 pg/mm,实验结果与案件受害者所述服药时间基本一致。结论 多根头发微分段分析技术可应用于药物辅助犯罪案例的调查,并可对服药时间进行大致判断。

【Abstract】 Objective To establish an analytical method of LC-MS/MS based on micro-segmentation analysis of multiple hairs, verify the detection of 20 benzodiazepines in 1mm hair, and finally use it for case detection analysis.Methods 5 hairs were cut into 1mm long segments each, and the corresponding segments were immersed and sonicated in an extract containing dithiothreitol, methanol, etc. Mobile phase A was 0.1% formic acid in water, and mobile phase B was acetonitrile. Data were collected using electrospray ion source positive ion mode in multiple reaction monitoring mode.Results The 20 benzodiazepines in multiple hairs had a good linear relationship(r > 0.99), detection limit of 0.2 ~ 5 pg/mm, minimum quantification limit of 0.5 to 20 pg/mm, the intro-day and inter-day precisions of 2.03 % to 13.81 %, the intro-day and inter-day accuracies of 87.98 % ~ 111.29 %, matrix effect of 71.15 % ~ 110.43 %, and extraction recovery of 69.34 % to 99.94 %. Using this method, hair samples were analyzed in volunteers taking a single dose of clonazepam for 20 days, and the detected location of clonazepam in 15 hairs was located in segment 6 ~ 11 from the hair root, with the concentration range of 1.06 ~ 3.45 pg/mm. By this method, the hair of the victims suspected of having taken sleeping pills in the case was analyzed. In 15 hairs, clonazepam was detected in segments 9 ~ 13 of the hair root. The quantitative results were 1.07 ~ 19.06 pg/mm. The experimental results were basically consistent with the medication time of the victim. Conclusion The microsegmentation analysis technique of multiple hairs can be applied to the investigation of drug-assisted crime cases,and can roughly estimate the medication time.

【基金】 国家重点研发计划项目分析公安部重点实验室专项基金项目(2021YFF0602504)
  • 【文献出处】 中国法医学杂志 ,Chinese Journal of Forensic Medicine , 编辑部邮箱 ,2024年06期
  • 【分类号】D919
  • 【下载频次】10
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