液相色谱-串联质谱法测定生活饮用水中磺胺类药物及其代谢物

发布时间：2018-02-27 01:13

本文关键词： 磺胺类抗生素及其代谢物固相萃取液相色谱-串联质谱生活饮用水　出处：《卫生研究》2015年04期 　论文类型：期刊论文

【摘要】：目的建立测定地表水、市政末梢水和自备井水源水中磺胺类药物及其代谢物的液相色谱-串联质谱法。方法比较不同固相萃取柱对生活饮用水中目标药物的提取效率,优化富集净化过程。样品调节p H至3.0,经MCX固相萃取柱净化,用高效液相色谱-串联质谱(LC-MS/MS)检测。C18柱(2.1 mm×100 mm,1.7μm)分离,以0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱;正离子多反应监测模式检测。目标药物使用基质外标法定量。结果 21种目标药物的线性范围为0.5~500ng/L,相关系数均大于0.99。方法定量限为0.03~0.63 ng/L,3个加标水平的回收率为50.1%~114.9%,相对标准偏差(RSD)为0.5%~15.0%。应用该方法对北京市部分自备井水源水、地表水和市政末梢水进行检测,共检出磺胺嘧啶、磺胺噻唑、磺胺吡啶、甲氧苄啶和磺胺甲嘧啶,其浓度为0.08~32.54 ng/L。结论该方法灵敏、简便,适用于生活饮用水中多种磺胺类药物及其代谢物残留的同时测定。
[Abstract]:Objective to establish a liquid chromatography-tandem mass spectrometry (LC-MS) method for the determination of sulfanilamides and their metabolites in surface water, municipal peripheral water and self-provided well water. Methods the extraction efficiency of target drugs in drinking water by different solid-phase extraction columns was compared. The sample was adjusted from pH to 3.0, purified by MCX solid-phase extraction column, and separated by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS). The sample was separated with 0.1% formic acid aqueous solution and acetonitrile as mobile phase. Results the linear range of 21 target drugs was 0.5 ~ 500ng / L, the correlation coefficient was greater than 0.99.The quantitative limit of the method was 0.03 ~ 0.63 ng / L, and the recoveries of the three standard adding levels were 50.1 ~ 114.9%, respectively. The relative standard deviation (RSD) is 0. 5 and 15. 0. The method is applied to some of the well water source water provided by Beijing. Sulfadiazine, sulfathiazole, sulfampyridine, trimethoprim and sulfamethazine were detected in surface water and municipal peripheral water. The concentration of sulfadiazine was 0.08 渭 g / L, 32.54 ng / L, respectively. Conclusion the method is sensitive and simple. It is suitable for simultaneous determination of sulfonamides and their metabolites in drinking water.
【作者单位】：北京市朝阳区疾病预防控制中心;北京市疾病预防控制中心北京市食物中毒诊断溯源技术北京市重点实验室;
【基金】：首都卫生行业发展专项(No.2011-7023-02)
【分类号】：R123.1

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