【摘要】 目的建立超高效液相色谱-串联质谱（UPLC-MS/MS）检测方法,测定饮用水中硝西泮、地西泮、奥沙西泮、氯氮卓、氯硝西泮5种常用苯二氮卓类药物。方法500 ml水样经MCX柱富集净化,ACQUITY BEH C₁₈（2.1 mm×100 mm,1.7μm）色谱柱分离,以甲醇-水为流动相梯度洗脱,采用电喷雾正离子源（ESI+）在多反应监测模式（MRM）下进行测定,外标法定量。结果 5种目标化合物在选定浓度范围内线性关系良好,相关系数（r²）均>0.999。方法的定量限（LOQ）为0.050⁰.500 ng/L,3个添加水平的加标回收率为78.2%¹08.0%,相对标准偏差≤12.4%（n=6）。利用该方法对96份饮用水样品进行分析,51份样品检出地西泮,浓度范围为<LOQ²9.92 ng/L;13份样品检出奥沙西泮,浓度范围为<LOQ⁹3.93 ng/L。结论本方法前处理简便、灵敏度高、重复性好,可用于饮用水样品中5种苯二氮卓类药物的定量检测。更多还原

【Abstract】 Objective A simultaneous determination method for five benzodiazepines（ nitrazepam, diazepam,oxazepam,chlordiazepoxide,clonazepam） in drinking water was developed using ultra performance liquid chromatographytandem mass spectrometry（ UPLC-MS/MS）. Methods Samples were concentrated and purified with MCX solid-phase extraction cartridge. The chromatographic separation was achieved using an ACQUITY BEH C₁₈（ 2. 1 mm × 100 mm,1. 7 μm） column with methanol and water as mobile phase. The targets were analyzed with ESI operating in positive multiple reaction monitoring（ MRM） mode. Quantification was performed by matrix-matched standard calibration. Results Satisfactory linearity（ r²> 0. 999） was obtained for all targets,with the limits of quantification（ LOQs） ranged in 0. 050-0. 500 ng/L. Average recoveries at three spiked levels were 78. 2 %-108. 0 %,with relative standard deviations（ RSDs） less than or equal to 12. 4%（ n = 6）. The developed method was used to analyze 96 drinking water samples,in which 51 samples were detected containing diazepam and 13 samples containing oxazepam. The concentrations were< LOQ-29. 92 ng/L and < LOQ-93. 93 ng/L,respectively. Conclusion The established method was simple,highly sensitive and with good repeatability,and could be applied in analysis of 5 benzodiazepines in drinking water.更多还原