QuEChERS-在线GPC-GC/MS联用法测定尿液中11种苯二氮卓类药物  

Determination of 11 benzodiazepine drugs in urine with QuEChERS-on line gel permeation chromatography-gas chromatography/mass spectrometry

作　　者：黄伟华[1] 夏祥[1] 胡美华[1] HUANG Wei-hua;XIA Xiang;HU Mei-hua(Nanchang Center for Disease Control and Prevention,Nanchang 330038)

机构地区：[1]南昌市疾病预防控制中心,南昌330038

出　　处：《分析试验室》2019年第1期43-46,共4页Chinese Journal of Analysis Laboratory

基　　金：江西省卫计委科技计划资助项目(20166035)资助

摘　　要：建立了QuEChERS法结合在线GPC-GC/MS联用对尿液中11种苯二氮卓类药物的分析方法。在NaCl作用下,尿液经乙腈提取后,采用QuEChERS前处理技术进行净化,提取液再通过在线GPC有效去除大分子化合物,经石英毛细管色谱柱DB-5MS (30 m×0. 25 mm×0. 25μm)分离,EI源选择离子监测模式下分析测定,外标法定量。结果表明:在优化条件下,11种苯二氮卓类药物的色谱峰分离良好,且各标准化合物的相关系数均大于0. 997,检出限为0. 06～10. 8 ng/mL。尿样在高、中、低3个浓度的加标回收率为81. 0%～100. 5%,相对标准偏差为3. 1%～6. 9%。方法已应用于尿液中这11种苯二氮卓类药物的检测。A method was established for the simultaneous determination of 11 benzodiazepine drugs in urine using on line gel permeation chromatography-gas chromatography/mass spectrometry coupled with QuEChERS.Under the salting out using NaCl,the samples were purified by QuEChERS after extracted with acetonitrile,and then the high molecular weight compounds were removed through on line GPC.The target compounds were separated by DB-5MS(30 m×0.25 mm×0.25 μm),analyzed by MS with EI under selected-ion monitoring(SIM)mode and external standard method.Under the optimized conditions,11 kinds of benzodiazepine drugs were successfully separated.The correlation coefficient of each target compounds was more than 0.997,and the detection limits ranged from 0.06 ng/m L to 10.8 ng/m L.The recoveries of 11 target compounds with the of low,middle and high concentration were in the range of 81.0 %-100.5 % with RSDs(n=5)of 3.1 %-6.9 %.The proposed method was simple,rapid and sensitive,and was suitable for the determination of 11 benzodiazepine drugs in urine.

关 键 词：QUECHERS 在线GPC-GC/MS 尿液 苯二氮卓类 药物 

分 类 号：R446[医药卫生—诊断学] O657.63[医药卫生—临床医学]