超高效液相色谱-串联质谱法同时检测环境水中5种苯二氮卓类镇静剂药物

Simultaneous determination of 5 benzodiazepine sedatives in environment water by liquid chromatography-tandem mass spectrometry

目的建立同时测定环境水中的地西泮、硝西泮、去甲西泮、奥沙西泮、氟胺安定等5种苯二氮卓类镇静剂的检测方法。方法 500 ml环境水样品以5.0 ml/min流速过HLB固相萃取柱富集、洗脱收集后,以D5-地西泮为内标,直接超高效液相色谱-串联质谱(UPLC-MS/MS)进样分析。采用Waters BEH C18柱(50 mm×2.1 mm,1.7μm),流动相为0.1%的甲酸水溶液和乙腈,梯度洗脱,流速:0.3 ml/min;质谱检测器采用ESI电离源,正离子多反应监测(MRM)扫描分析。结果地西泮、硝西泮、去甲西泮、奥沙西泮、氟胺安定等5种苯二氮卓类镇静剂药物在0.2 ng/L^200 ng/L内,线性关系良好(r值为0.996 9~0.999 6),最低检出限为0.1 ng/L^0.4 ng/L,最低定量限为0.3 ng/L^1.3 ng/L;在生活饮用水中添加5种镇静剂浓度分别为2.0 ng/L、20.0 ng/L、100.0 ng/L时,平均回收率为88.3%~109.2%,相对标准偏差为2.2%~9.8%。结论该方法快速、灵敏、准确度高,适用于生活饮用水中多种苯二氮卓类镇静剂的含量监测。

Objective To establish a method for simultaneous determination of 5 benzodiazepine sedatives（ Diazepam,Nitrazepam,Nordazepam,Oxazepam,and Flurazepam） in water. Methods 500 ml water was concentrated by HLB solid phase extraction column at a speed of 5. 0 ml/min,and then was analyzed by ultra-high performance liquid chromatography-tandem mass spectrometry（ UPLC-MS/MS） directly using D5-Diazepam as internal standard. Separation of the compounds was carried out on an Acquity UPLC BEH C18 column（ 50 mm × 2. 1 mm,1. 7 μm）,with a gradient elution of 0. 1% formic acid water solution and acetonitrile at a flow rate of 0. 3 ml/min. The mass spectrometer detector took ESI ionization source,and positive ion multiple reaction monitoring（ MRM） carried out scan analysis. Results Good linearity was obtained when the concentrations of the 5 benzodiazepine sedatives were within 0. 2 ng/L-200 ng/L,with correlative coefficient（ r） of 0. 996 2-0. 999 8. The lowest limit of detection（ LOD） was within 0. 1 ng/L-0. 4 ng/L and the lowest limit of quantification was within 0. 3 ng/L-1. 3 ng/L.When the concentrations of 5 sedatives in drinking water were 2. 0 ng/L and 20. 0 ng/L and 100. 0 ng/L,the average recovery was within 88. 3%-109. 2%,with the relative standard deviation of 2. 2%-9. 8%. Conclusion The method is rapid,sensitive and accurate. It is suitable for monitoring the content of benzodiazepine sedatives in drinking water.