毛细管固相微萃取-液质联用测定血浆中5种新型滥用药物

摘要

目的：建立毛细管固相微萃取-超高效液相色谱-串联质谱( UPLC-MS/MS)法测定血浆中新型滥用药物。方法取含药物成分的血浆样品1 mL,加入硼砂缓冲液2 mL后吸入注射器中,与内壁固定有DB-1701毛细管柱的不锈钢针头连接,置于注射泵,以300μL·min-1流速排出样品,乙腈50μL洗脱2 min,采用UPLC-MS/MS梯度洗脱-正离子多反应监测扫描测定洗脱液中药物成分,并对实际样品进行检验。结果血浆中盐酸可待因、盐酸曲马多、地芬诺酯、地西泮、三唑仑等5种新型滥用药物回收率为69.2%~81.7%,RSD<10%,检测限<25 ng·mL-1,26起案例样品中检出7例。结论采用毛细管固相微萃取方法简便,快速,与UPLC-MS/MS技术结合可用于血浆中新型滥用药物的快速筛查。%Objective To establish a method for determination of new abused drugs in plasma by using ultra-high performance liquid chromatography tandem mass spectrometry ( UPLC-MS/MS ) combined with in-tube solid-phase microextraction. Methods 2 mL of borax buffer was added to 1 mL of plasma with drugs. Then,the mixture was withdrawn into a syringe connected to a stainless steel needle welded with DB-1701 capillary column. 50 μL acetonitrile was used as elution solvent at the flow rate of 300 μL·min-1 for 2 min. Subsequently,the drugs on elute were determined by using UPLC-MS/MS in positive mode with multiple reaction monitoring( MRM) to determine drug concentration in human plasma samples. ResultsThe recoveries rates of the five abused drugs ( codeine hydrochloride, tramadol, diphenoxylate hydrochloride, diazepam, and triazolam) in plasma were between 69. 2% -81. 7% with the RSDs less than 10%. LODs of the drugs were less than 25 ng·mL-1 . Seven out of the 26 plasma samples were determined positive. Conclusion The in-tube SPME method coupled to UPLC-MS/MS is simple, rapid, and environmental friendly, which is suitable for the the rapid screening of the new abused drugs.