超高效液相色谱-串联质谱法测定毛发中4种苯丙胺类兴奋剂含量的不确定度评估  

Uncertainty Evaluation for the Determination of Four Amphetamine-type Stimulants in Hair by Ultra-performance Liquid Chromatography-tandem Mass Spectrometry

作　　者：胡骏杰 马文俊 刘飞 朱军 张润生[4] HU Jun-jie;MA Wen-jun;LIU Fei;ZHU Jun;ZHANG Run-sheng(Judicial Expertise Center,Jining Medical University,Jining 272067,China;College of Forensic Medicine and Laboratory Medicine,Jining Medical University,Jining 272067,China;State Key Laboratory of Analytical Chemistry for Life Science,School of Chemistry and Chemical Engineering,Nanjing Universit,Nanjing 210023,China;Center for Evidence Authentication,Sshanghai Municipal Public Security Bureau,Shanghai 200083,China)

机构地区：[1]济宁医学院司法鉴定中心,山东济宁272067 [2]济宁医学院法医学与医学检验学院,山东济宁272067 [3]南京大学化学化工学院,生命分析化学国家重点实验室,江苏南京210023 [4]上海市公安局物证鉴定中心,上海200083

出　　处：《化学试剂》2021年第8期1111-1116,共6页Chemical Reagents

基　　金：国家自然科学基金资助项目(21904049);国家级大学生创新训练计划项目(201910443005);济宁医学院大学生创新训练计划项目(cx2019061);山东省高等学校科技计划项目(J18KB047);济宁医学院教师扶持基金资助项目(JYFC2018FY005)。

摘　　要：建立了毛发中4种苯丙胺类兴奋剂的超高效液相色谱-串联质谱外标定量检测方法,并对该方法进行了不确定度评估。通过分析整个实验过程,从标准溶液配制、样品配制、线性拟合、样品处理过程、基质效应等方面确定不确定度来源,量化各不确定度分量,并进行合成与扩展。结果表明,毛发中苯丙胺类兴奋剂测定结果不确定度最主要的来源为标准曲线拟合。基于司法鉴定工作需要,特别给出了毛发中4种苯丙胺类兴奋剂在成瘾认定含量阈值(0.2 ng/mg)处完整的不确定度报告,各物质扩展不确定度为0.024 0~0.035 6 ng/mg。该评估结果可为吸毒成瘾认定案件的法医鉴定工作提供有效参考信息。A method was developed for quantitative detection of four amphetamine-type stimulants(ATSs)in hair by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)combined with the external standard,and the uncertainty of the method was evaluated.Through the analysis of the entire experimental process,the uncertainty source is determined from the standard solution preparation,sample preparation,linear fitting,sample processing process,matrix effect,etc.Each uncertainty component is quantified,synthesized and expanded.The results showed that the main source of uncertainty in the determination of ATSs in hair was standard curve fitting.Based on the needs of forensic appraisal,A complete uncertainty report of the four ATSs in the hair at the addiction determination threshold(0.2 ng/mg)was especially given,and the expanded uncertainty of each substance was 0.0240~0.0356 ng/mg.The evaluation results can provide effective reference information for the forensic identification of drug addiction cases.

关 键 词：超高效液相色谱-串联质谱 毛发 苯丙胺类兴奋剂 外标定量 不确定度 吸毒成瘾认定 

分 类 号：O657.63[理学—分析化学]