固相萃取-超高效液相色谱-串联质谱法测定水中5种常用苯二氮卓类药物
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(1.首都医科大学公共卫生学院,北京 100069;2.北京市疾病预防控制中心 食物中毒诊断溯源 技术北京市重点实验室,北京 100013;3.北京市预防医学研究中心,北京 100013)

作者简介:

张昕 女 硕士生 研究方向为食品安全检测 E-mail:f_zhangxin@163.com通信作者:邵兵 男 研究员 研究方向为化学污染检测 E-mail:shaobingch@sina.com

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国家自然科学基金(21677019);首都卫生发展科研专项项目(2014-1-3011)


Determination of five benzodiazepines in water by solid-phase extraction and ultra performance liquid chromatography-tandem mass spectrometry
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(1.School of Public Health, Capital Medical University, Beijing 100069, China; ;2.Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Center for Disease Prevention and Control, Beijing 100013, China;3.Beijing Research Center for Preventive Medicine, Beijing 100013, China)

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    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,1.7 μm)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0.050~0.500 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

    Abstract:

    Objective A simultaneous determination method for five benzodiazepines (nitrazepam, diazepam, oxazepam, chlordiazepoxide, clonazepam) in drinking water was developed using ultra performance liquid chromatography-tandem 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

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张昕,张晶,邵兵.固相萃取-超高效液相色谱-串联质谱法测定水中5种常用苯二氮卓类药物[J].中国食品卫生杂志,2017,29(6):684-689.

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  • 收稿日期:2017-08-22
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  • 在线发布日期: 2018-01-29
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