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
谢琳溪 1薛鼎昌 2郭兆辰 3任飞 2李婧 2贠克明 4尉志文 4张潮 4辛国斌5
作者信息
- 1. 山西医科大学,山西 太原 030606;太原市公安局,山西 太原 030000
- 2. 太原市公安局,山西 太原 030000
- 3. 内蒙古科技大学,内蒙古自治区 包头 014017
- 4. 山西医科大学,山西 太原 030606
- 5. 北京市公安局,北京 102611
- 折叠
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 种苯二氮䓬类药物在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 种苯二氮䓬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 micro-segmentation analysis technique of multiple hairs can be applied to the investigation of drug-assisted crime cases,and can roughly estimate the medication time.
关键词
毒物分析/毛发微分段/液质联用仪/苯二氮䓬类/药物辅助犯罪Key words
Toison analysis/Hair differential segment/Liquid mass instrument/Benzodiazepine/Drug-assisted crime引用本文复制引用
出版年
2024
NETL
NSTL
万方数据