毛细管固相微萃取/UPLC-MS/MS测定血浆中毒品成分  

Determination of drugs in human plasma by in-tube solid-phase microextraction coupled to liquid chromatography tandem mass spectrometry

作　　者：王毅 刘子秋 王炯[2] 

机构地区：[1]贵阳市公安司法鉴定中心,贵州贵阳550007 [2]公安部物证鉴定中心,北京100038

出　　处：《中国法医学杂志》2014年第4期319-321,325,共4页Chinese Journal of Forensic Medicine

基　　金：贵阳市科技计划项目[2012103]98号;贵州省优秀科技教育人才省长专项资金项目(2011)23号

摘　　要：目的建立毛细管固相微萃取UPLC-MS／MS测定血浆中毒品的方法，并用于实际样品分析。方法取含毒品成分的血浆样品lmL，加入2mL硼砂缓冲液后吸入注射器中，联接内壁上固定有DB-1701毛细管柱的不锈钢针头，流动注射泵以300μL／min流速使样品全部排出，lmL纯水冲洗，50μL乙腈洗脱2min，UPLC-MS／MS梯度洗脱-正离子一多反应监测测定洗脱液毒品成分，并对28例案件样品进行分析。结果血浆中毒品回收率为64．5％～82．1％，RSD〈10％，LOD〈40ng／mL，28份样品中检出19例。结论采用毛细管固相微萃取（in-tubeSPME），方法快速、简棒、环保．与UPLC-MS／MS桔术结合可府用干血浆中毒品的快速筛查。Objective To establish a method for determination of abused drugs in plasma by using in- tube solid-phase microextraction combined with liquid chromatography tandem mass spectrometry （UPLC- MS/MS）. Methods 2mL of sodium borate buffer was added into 1 mL of plasma, taken into a sampler, con- nected with stainless steel needle which welded with DB-1701 capillary column. The eject speed was set to 300μL/min. After l mL water and 50μL of acetonitrile were used for eluting the analytes from the column, UPLC-MS/MS condition was set to gradient elution coupled with multiple reaction monitoring for drug deter- minition. This method was used in detecting drugs in blood samples from 28 real cases. Results The recoveries of abused drugs in plasma were between 69.2% - 81.7 % with the RSD less than 10%. LOD of the drugs were below 40 ng/mL, 19 out of the 28 cases were detected as positive. Conclusion The intube SPME method is simple, rapid, environmentally friendly. Coupled to UPLC-MS/MS, it is suitable for fast screening of the drugs in blood samples.

关 键 词：法医毒物分析 毛细管固相微萃取 UPLC-MS/MS 血浆 毒品 

分 类 号：D919[医药卫生—法医学]