液相色谱-串联质谱法测定干血点中晕车药及代谢物  

Determination of Motion Sickness Drugs and Metabolite in Dried Blood Spots by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：吴浩天 陈学国[1,2] 田露 杜政达 WU Hao-tian;CHEN Xue-guo;TIAN Lu;DU Zheng-da(School of Forensic Science,Criminal Investigation Police University of China,Shenyang 110854,China;Key Laboratory of Forensic Toxicology,Ministry of Public Security,People’s Republic of China,Beijing 100192,China)

机构地区：[1]中国刑事警察学院刑事科学技术学院,辽宁沈阳110854 [2]法庭毒物分析公安部重点实验室,北京100192

出　　处：《分析测试学报》2024年第6期939-944,共6页Journal of Instrumental Analysis

基　　金：法庭毒物分析公安部重点实验室开放课题(2023FTDWFX03);2023年度中国刑事警察学院中央高校基本科研业务费项目(C2023009);2023年度教育厅基本科研项目(JYTMS20231413);2023年度研究生创新能力提升项目(2023YCYB51);公安部科技计划项目(2023JSYJC22)。

摘　　要：该文建立了干血点(DBS)中东莨菪碱、阿托品、茶碱、地芬尼多、苯海拉明及二苯甲酮的液相色谱-串联质谱检测方法。取20μL血液制备干血点,以甲醇-乙腈(体积比8∶2)为溶剂进行超声提取,采用Thermo Gold ODS(150 mm×2.1 mm,5μm)色谱柱进行分离,以甲醇-5 mmol/L乙酸铵溶液(含0.2%冰乙酸,pH 4.0)为流动相梯度洗脱,在正离子电离方式下采用多反应监测模式进行测定,以外标法定量。结果表明:干血点中6种目标物在一定的质量浓度范围内线性关系良好,相关系数(r^(2))均不小于0.9930,检出限为3~30 ng/mL,定量下限为10~100 ng/mL;在低、中、高3个加标水平下,6种目标物的平均回收率为88.8%~108%,日间和日内相对标准偏差均小于15%。该方法操作简便、快捷,准确度和灵敏度高,已成功应用于1例地芬尼多中毒者的检测,为晕车药中毒案例的测定提供了新方法。In this paper,a liquid chromatography-tandem mass spectrometry(LC-MS/MS)method was developed for the determination of scopolamine,atropine,diphenidol,theophylline,diphen⁃hydramine and benzophenone in dried blood spots(DBS).A dried blood spot was prepared by taking 20μL of blood,extracted by methanol-acetonitrile(8∶2,volume ratio)as solvent by ultrasonica⁃tion,separated on a Thermo Gold ODS(150 mm×2.1 mm,5μm)column,with methanol-5 mmol/L ammonium acetate solution(containing 0.2%glacial acetic acid,pH 4.0)was used as the mobile phase for gradient elution,and then measured in multiple reaction monitoring(MRM)mode of the positive-ion mode,and quantified by external standard method.The results showed that the linearity of the six targets in dried blood spots was good within a certain mass concentration range,and the cor⁃relation coefficients(r^(2))were not less than 0.9930.The limits of detection(LODs)ranged from 3 to 30 ng/mL,and the limits of quantification(LOQs)ranged from 10 to 100 ng/mL.The average recov⁃eries of the six targets ranged from 88.8%to 108%at low,medium and high concentration levels,with the inter-day and intra-day relative standard deviations were less than 15%.The method was sim⁃ple and fast,with high accuracy and sensitivity,and has been successfully applied to the detection of one case of difenidol poisoning,which provides a new method for the determination of cases of mo⁃tion sickness drug poisoning.

关 键 词：干血点 晕车药 代谢物 液相色谱-串联质谱法 

分 类 号：O657.7[理学—分析化学] D919.4[理学—化学]