【摘要】 目的:建立人血浆中苯二氮类液相色谱-大气压化学源-串联质谱(LC-APCI-MS/MS)的检测方法。方法:血浆中的苯二氮类药物用乙醚液-液萃取,采用AgilentZorbaxSB-C18(2.1mm×150mm,5μm)柱子,柱温25℃,流动相为乙腈-0.1%甲酸溶液(35∶65,V/V),流速0.4mL·min-1,进样量10μL;大气压化学电离源(APCI),正离子检测,采用多反应监测(multiple reaction monitoring,MRM)方式进行定量分析。结果:7种苯二氮类药物的最小检测限(LOD)在0.33～1.12ng.mL-1之间,浓度在1.01～675ng.mL-1范围内线性良好(r≥0.9923),平均萃取回收率在70.1%～88.7%之间,日内、日间精密度RSD≤6%(n=5)。结论:该方法专属性强、灵敏及准确,可以适用于法庭与临床毒物分析。更多还原

【Abstract】 Objective:To develop a method for determination of benzodiazepine drugs in human plasma by liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry/mass spectrometry(LC-APCI-MS/MS).Methods:Benzodiazepine drugs were extracted from plasma samples by aether and separation was carried out on Agilent Zorbax SB-C18 column(2.1 mm×150 mm,5 μm)at 25 ℃,with acetonitrile-0.1% formic acid(35∶65,V/V)as mobile phase at flow rate of 0.4 mL·min-1,the injection volume was 10 μL;atmospheric pressure chemical ionization(APCI)source was applied and operated in positive ion mode,and multiple reaction monitoring(MRM)mode was used to quantify benzodiazepine drugs.Results:The detection limits(LOD)of 7 benzodiazepine drugs were within 0.33-1.12 ng·mL-1.The calibration curve in the concentration range of 1.01-675 ng·mL-1 showed a good linear(r≥0.9923).The average extraction recoveries were within 70.1%-88.7%.Intra-day RSD and inter-day RSD were less than 6%(n=5).Conclusion:This method is specific,sensitive and accurate,and can be used to detect benzodiazepine drugs in forensic and clinical analytic toxicology.更多还原