在线固相萃取/液质联用法检测血液和尿液中10种巴比妥类药物  

Analysis of 10 barbiturates in blood and urine by liquid chromatography-tandem mass spectrometer with on-line solid phase extraction

作　　者：莫静[1] 黄克建[2] 罗轩[1] 刘晓峰 杨宁[2] 姚苏芝 王怡媛 林翠梧[1] MO Jing;HUANG Ke-jian;LUO Xuan;LIU Xiao-feng;YANG Ning;YAO Su-zhi;WANG Yi-yuan;LIN Cui-wu(College of Chemistry and Chemical Engineering, Guangxi University, Nanning 530004, China;Evidence Identification Center,Guangxi Zhuang Autonomous Region PublicSecurity Department, Nanning 530012, China)

机构地区：[1]广西大学化学化工学院,广西南宁530004 [2]广西壮族自治区公安厅物证鉴定中心,广西南宁530012

出　　处：《广西大学学报（自然科学版）》2018年第6期2407-2414,共8页Journal of Guangxi University（Natural Science Edition）

基　　金：广西公安科学研究与技术开发计划立项项目(GAT2016-14)

摘　　要：文中建立了在线固相萃取/液相色谱—三重串联四极杆质谱(on-line SPE/LC-MS/MS)方法同时测定血液和尿液中10种巴比妥类药物。样品用乙腈沉淀蛋白,经在线固相萃取柱(HLB)富集纯化,以Poroshell 120EC-C18柱(2. 1 mm×50 mm,1. 9μm)为分析柱,乙腈—水为流动相进行梯度洗脱。电离模式为电喷雾电离负模式(ESI-),扫描方式为多反应监控模式(MRM),定量方法采用外标法。结果表明,10种化合物在各自质量浓度范围内线性关系良好(权重因子1/x),相关系数为0. 998 8～0. 999 5,方法检出限(MDL)和定量限(LOQ)分别为10. 0～20. 0 ng/m L和20. 0～50. 0 ng/m L,回收率为95. 8%～109. 5%,相对标准偏差(RSD)为0. 5%～3. 8%(n=6)。检测方法操作简单,耗时短,检测灵敏度高且结果准确,能够满足血液和尿液样品中10种化合物同时快速筛查和准确定量。A method of liquid chromatography-tandem mass spectrometry(LC-MS/MS)with on-line solid phase extraction(on-line SPE)for the simultaneous determination of 10 barbiturates in blood and urine was developed and validated.The samples were treated with acetonitrile,and then purified by a column with polymer of hydrophilic-lipophilic balance(HLB).The samples were eluted on a Poroshell 120 EC-C18 column by acetonitrile and water.The analysis was detected in multiple-reaction monitoring(MRM)mode under negative electrospray ionization mode(ESI-)and quantified by external standard method.The results show that the correlation coefficients are 0.9988~0.9995 within the investigated mass concentration ranges of the 10 barbiturates.The LODs vary from 10.0 ng/mL to 20.0 ng/mL,and the LOQs vary from 20.0 ng/mL to 50.0 ng/mL.The recoveries at different spiked levels in blood and urine range from 95.8%to 109.5%,and RSDs range from 0.5%to 3.8%(n=6).The method is simple,reliable and highly sensitive for the rapid detection and accurate quantification of the 10 barbiturates in blood and urine.

关 键 词：在线固相萃取 液相色谱—串联质谱 巴比妥类 生物样品 

分 类 号：O656.3[理学—分析化学]