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作 者:纪佼佼 徐多麒 向平 严慧 沈敏 JI Jiao-jiao;XU Duo-qi;XIANG Ping;YAN Hui;SHEN Min(Shanghai Key Laboratory of Forensic Medicine,Key Laboratory of Forensic Science,Ministry of Justice,Shanghai Forensic Service Platform,Academy of Forensic Science,Shanghai 200063,China;School of Basic Medical Sciences,Fudan University,Shanghai 200032,China)
机构地区:[1]司法鉴定科学研究院上海市法医学重点实验室司法部司法鉴定重点实验室上海市司法鉴定专业技术服务平台,上海200063 [2]复旦大学基础医学院,上海200032
出 处:《法医学杂志》2023年第2期151-160,共10页Journal of Forensic Medicine
基 金:国家自然科学基金资助项目(81772022);司法部司法鉴定重点实验室资助项目;上海市法医学重点实验室资助项目(21DZ2270800);上海市司法鉴定专业技术服务平台资助项目。
摘 要:目的建立一种基于单根头发微分段技术的LC-MS/MS分析方法,并对42种精神活性物质在0.4 mm头发节段中的检测进行验证。方法将每根头发剪成0.4 mm长的片段,超声提取,并在含二硫苏糖醇的提取液中浸泡。流动相A为含20 mmol/L乙酸铵、0.1%甲酸、5%乙腈的水溶液,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。结果单根头发中42种精神活性物质在各自线性范围内线性关系良好(r>0.99),检出限为0.2~10 pg/mm,最低定量限为0.5~20 pg/mm,日内、日间精密度为1.5%~12.7%,日内、日间准确度为86.5%~109.2%,提取回收率为68.1%~98.2%,基质效应为71.3%~111.7%。应用该方法对单次服用唑吡坦28 d的志愿者头发样本进行分析,5根头发中唑吡坦的检出位置位于近根端1.08~1.60 cm,浓度范围为0.62~20.5 pg/mm。结论单根毛发微分段分析技术可应用于药物辅助性犯罪案件的调查。Objective To establish an LC-MS/MS method based on single hair micro-segmental technique,and verify the detection of 42 psychoactive substances in 0.4 mm hair segments.Methods Each piece of single hair was cut into 0.4 mm segments and extracted by sonication and the segments were immersed in dithiothreitol-containing extraction medium.Mobile phase A was the aqueous solution containing 20 mmol/L ammonium acetate,0.1%formic acid,and 5%acetonitrile.Mobile phase B was acetonitrile.An electrospray ionization source in positive ion mode was used for data acquisition in multiple reaction monitoring(MRM)mode.Results The 42 psychoactive substances in hair had a good linear relationship within their respective linear ranges(r>0.99),the limits of detection were 0.2-10 pg/mm,the limits of quantification were 0.5-20 pg/mm,the intra-day and inter-day precisions were 1.5%-12.7%,the intra-day and inter-day accuracies were 86.5%-109.2%,the recovery rates were 68.1%-98.2%,and the matrix effects were 71.3%-111.7%.The method was applied to hair samples collected from one volun teer at 28 d after a single dose of zolpidem,with zolpidem detected in 5 hairs was 1.08-1.60 cm near the root tip,and the concentration range was 0.62-20.5 pg/mm.Conclusion The micro-segmental technique of single hair analysis can be applied to the investigation of drug-facilitated sexual assault cases.
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