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 C_(18)(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(r^2)均>0.999。方法的定量限(LOQ)为0.050~0.500 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<LOQ^29.92 ng/L;13份样品检出奥沙西泮,浓度范围为<LOQ^93.93 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。
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 C_（18）（ 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.
出处
《中国食品卫生杂志》
2017年第6期684-689,共6页
Chinese Journal of Food Hygiene
基金
国家自然科学基金(21677019)
首都卫生发展科研专项项目(2014-1-3011)
关键词
饮用水
苯二氮卓类药物
固相萃取
超高效液相色谱-串联质谱法
违法添加
食品安全
Drinking water
benzodiazepines
solid-phase extraction
ultra performance liquid chromatography-tandemmass spectrometry
adulterant
food safety
