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.