论文部分内容阅读
目的建立超高效液相色谱-串联质谱法测定人尿液中8种苯二氮?类及3种非苯二氮?类药物的浓度。方法尿液样品采用二氯甲烷∶正己烷∶乙酸乙酯(5∶4∶1)进行萃取,Waters ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm,1.8μm)进行分离,乙腈-0.1%氨水溶液为流动相进行梯度洗脱,流速为0.2 m L·min?1,通过电喷雾离子源,多重反应监测正离子模式进行检测。结果 11种被分析物在所测浓度范围内呈现良好的线性关系,相关系数均>0.99,除右佐匹克隆检测限为0.5 ng·m L?1,其他物质检测限为0.01~0.02 ng·m L?1,11种被分析物的日内、日间RSD均<15.0%(n=5),提取回收率为68.8%~115.0%,基质效应为0.85~1.14。结论该方法快速、灵敏、准确,适用于同时检测人尿中8种苯二氮?类及3种非苯二氮?类药物浓度。
OBJECTIVE To establish a method for the determination of 8 benzodiazepines and 3 non-benzodiazepines in human urine by ultra performance liquid chromatography-tandem mass spectrometry. Methods Urine samples were extracted with dichloromethane: n-hexane: ethyl acetate (5: 4: 1) and separated on a Waters ACQUITY UPLC HSS T3 column (2.1 mm × 100 mm, 1.8 μm) The gradient elution was carried out with mobile phase at a flow rate of 0.2 m L · min -1. Electrospray ionization (ESI) and multi-reaction monitoring of positive ion mode were carried out. Results The 11 analytes showed a good linearity within the range of the measured concentration, the correlation coefficient was> 0.99, the detection limit of dezocinil was 0.5 ng · m L -1, and the detection limit of other substances was 0.01-0.02 ng · The RSDs of intra-day and inter-day were all less than 15.0% (n = 5) for the 11 analytes. The recoveries ranged from 68.8% to 115.0%. The matrix effects ranged from 0.85 to 1.14. Conclusion The method is rapid, sensitive and accurate and suitable for the simultaneous determination of 8 benzodiazepines and 3 non-benzodiazepines in human urine.