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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1mL,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,1mL纯水冲洗,50μL乙腈洗脱2min,UPLC-MS/MS梯度洗脱-正离子-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<40 ng/mL,28份样品中检出19例。结论采用毛细管固相微萃取(in-tube SPME),方法快速、简捷、环保,与UPLC-MS/MS技术结合可应用于血浆中毒品的快速筛查。
OBJECTIVE To establish a capillary UPLC-MS / MS method for the determination of drugs in plasma and to analyze the actual samples. Methods 1 mL plasma samples containing drug components were taken, and 2 mL borax buffer was added to the syringe. Stainless steel needles with DB-1701 capillary column were attached to the inner wall of the syringe. The flow injection syringe was used to remove all the samples at a flow rate of 300 μL / Flushing, 50μL acetonitrile for 2min, UPLC-MS / MS gradient elution-positive ion-multiple reaction monitoring of elution drug components, and 28 cases of samples were analyzed. Results The recovery rate of plasma drug was 64.5% -82.1% with RSD <10% and LOD <40 ng / mL, and 19 samples were detected in 28 samples. Conclusion The method of capillary solid phase microextraction (in-tube SPME) is rapid, simple, and environmentally friendly and can be applied to the rapid screening of plasma drugs in combination with UPLC-MS / MS.