摘要
目的应用三重四极杆串联质谱建立毛发中10种毒品及其代谢物的灵敏、准确、快速分析方法,解决实际毛发样本中毒品的鉴定。方法毛发经冷冻研磨和超声提取后,用Restek Allure PFPP柱(100 mm×2.1mm,5μm)分离,流动相为含20 mmol/L乙酸铵、0.1%甲酸和5%乙腈的水溶液和乙腈,采用电喷雾离子源和分时间段扫描,在多反应监测(multiple reaction monitoring,MRM)模式下采集数据。结果吗啡等10种毒品及其代谢物在线性范围内线性关系良好(R2>0.995),检测限为0.5~6 pg/mg,定量限为2.5~10 pg/mg,准确度为89.1%~114.6%,日内精密度为0.2%~11.7%,日间精密度为4.0%~15.8%,基质效应为89.4%~118.4%,提取回收率为63.6%~112.1%。在196份实际毛发样本中检出阳性共20例。结论分时间段扫描法稳定性好、灵敏度高,可实现高通量检测,适用于法医毒物实验室对真实毛发中毒品的鉴定。
Objective To establish a sensitive,accurate and rapid detection method for 10 drugs and metabolites in hair with triple quadrupole tandem mass spectrometry,addressing the identification of drugs in real hair samples.Methods After cryogenic grinding and ultrasonic extraction,hair was separated by Restek Allure PFPP column(100 mm×2.1 mm,5μm).The mobile phase A was 20 mmol/L ammonium acetate,0.1%formic acid and 5%acetonitrile aqueous solution.The mobile phase B was acetonitrile.An electrospray ionization source was used for data acquisition in scheduled MRM mode.Results The method showed good linearity for all analytes within the validated range(R?>0.995),with the limits of detection ranging from 0.5 to 6 pg/mg,the limits of quantification ranging from 2.5 to 10 pg/mg.Accuracy ranged from 89.1%to 114.6%,with intra-day precision ranging from 0.2%to 11.7%,inter-day precision ranging from 4.0%to 15.8%.the matrix effects ranging from 89.4%to 118.4%,the recoveries ranging from 63.6%~112.1%.Totally 20 cases were detected positive in 196 actual hair samples.Conclusion The time-scheduled scanning method exhibits high stability and sensitivity,enabling high-throughput detection,and is suitable for forensic toxicology laboratoriestoidentifydrugs in hair.
作者
林梅婷
朱雪妍
李剑
窦全露
王鑫
向平
赵君博
Lin Meiting;Zhu Xueyan;Li Jian;Dou Quanlu;Wang Xin;Xiang Ping;Zhao Junbo(Shanghai Key Laboratory of Forensic Science,Key Laboratory of Forensic Medicine,Ministry of Justice,Shanghai Forensic Service Platform,Academy of Forensic Science,Shanghai 200063,China;School of Pharmacy,Shenyang Pharmaceutical University,Shenyang 116023,China;Hangzhou Puyu Technology Development Co,Ltd,Hangzhou 310000,China)
出处
《中国法医学杂志》
2025年第3期330-337,共8页
Chinese Journal of Forensic Medicine
基金
国家重点研发计划(2022YFC3300903)。
关键词
毛发
毒品
三重四极杆串联质谱
分时间段扫描
Hair
Drug
Triple quadrupole tandem mass spectrometry
Scheduled MRM mode
