摘要
目的建立指甲中甲基苯丙胺和苯丙胺的冷冻研磨结合高效液相色谱-串联质谱(LC-MS/MS)检测方法。方法样品经冷冻研磨处理,采用甲醇提取,应用高效液相色谱法分离,采用电喷雾离子源(ESI)、正离子模式扫描,多反应监测模式(MRM)检测,以保留时间和两对特征离子定性,以外标标准曲线法定量。结果指甲破碎方式中使用冷冻研磨处理的提取效果最好。甲基苯丙胺和苯丙胺均在0.2~25ng/mg范围内线性关系良好,相关系数分别为0.9991和0.9988,检出限均低于0.05ng/mg,定量限均为0.2ng/mg;提取回收率均高于85%,日内及日间精密度均小于10%。结论本方法快速、灵敏、准确,可应用于指甲中甲基苯丙胺、苯丙胺成分的定性定量检测。
Objective To develop and validate a rapid and sensitive method for simultaneous determination of methamphetamine and amphetamine in nail through frozen grinding coupled with high performance liquid chromatographymass spectrometry(HPLC-MS/MS).Methods The sampling nails were treated through frozen grinding and extracted with methanol,successively analyzed into high performance liquid chromatography(HPLC)coupling to AB QTRAP 4000 tandem mass spectrometry under the conditions of positive electrospray ionization mode(ESI+)and multiple reaction monitoring(MRM).Methamphetamine and amphetamine were qualitatively analyzed with their respective retention time and two characteristic ion pairs,with the external standard curve method being used for quantifi cation.Results The frozen grinding is the best treatment for the nail to extract effectively.The calibration curves were linear within the range of 0.2~25ng/mg for both methamphetamine and amphetamine,with their respective linear c oeffi cients be ing 0.9997 and 0.9968,the limits of detection being less than 0.05ng/mg,and the limits of quantifi cation lowering to 0.2ng/mg.A recovery greater than 85%was obtained from the method,with the inter-and intra-day RSD less than 10%.Conclusions The method is rapid,sensitive and accurate,suitable for determination of methamphetamine and amphetamine in nail samples.
作者
赵绪龙
马广鹏
武继锋
刘海燕
栾玉静
王爱华
ZHAO Xulong;MA Guangpeng;WU Jifeng;LIU Haiyan;LUAN Yujing;WANG Aihua(Institute of Criminal Science and Technology of Jinan Public Security Bureau,Jinan 250000,China;Institute of Forensic Science,Ministry of Public Security,Beijing 100038,China)
出处
《刑事技术》
2020年第6期601-605,共5页
Forensic Science and Technology
基金
中央级公益性科研院所基本科研业务费专项资金项目(2019JB042)。
