色谱

色谱 ›› 2015, Vol. 33 ›› Issue (7): 730-739.DOI: 10.3724/SP.J.1123.2015.03004

• 研究论文 • 上一篇    下一篇

超高效液相色谱-电喷雾串联质谱法测定生活饮用水中49种药物及5种代谢物

王硕1, 张向明1, 张晶2, 邵兵2, 李书明1   

  1. 1. 朝阳区疾病预防控制中心, 北京 100021;
    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
  • 收稿日期:2015-03-16 出版日期:2015-07-08 发布日期:2015-07-27
  • 通讯作者: 李书明
  • 基金资助:

    首都卫生行业发展专项(2011-7023-02).

Determination of 49 drugs and 5 metabolites in drinking water samples using ultra-high performance liquid chromatography- electrospray ionization tandem mass spectrometry

WANG Shuo1, ZHANG Xiangming1, ZHANG Jing2, SHAO Bing2, LI Shuming1   

  1. 1. Chaoyang District Center for the Disease Control and Prevention, Beijing 100021, China;
    2. Beijing Key Laboratory of Diagnostic and Traceability Technologies for the Food Poisoning, Beijing Center for the Disease Control and Prevention, Beijing 100013, China
  • Received:2015-03-16 Online:2015-07-08 Published:2015-07-27

PDF

136

被引次数

10

摘要：

建立了超高效液相色谱-电喷雾串联质谱(UPLC-ESI MS/MS)分析生活饮用水中54种药物的方法。采用HLB固相萃取柱对水样中的目标化合物进行富集净化,以5 mL甲醇洗脱;洗脱液用氮气吹至近干,用0.4 mL 0.1%甲酸水溶液定容,上机分析;ACQUITY UPLCTMBEH C18柱用作色谱分离,以0.1%甲酸水溶液-甲醇为流动相进行梯度洗脱;多反应监测(MRM)模式进行检测;目标药物使用基质外标法定量。54种药物在自备井水、市政末梢水和地表水中的加标回收率分别为58.7%~104.4%、53.1%~109.5%和50.7%~118.8%,相对标准偏差(n=6)分别为0.3%~12.8%、1.0%~15.5%和0.4%~19.3%;方法定量限为0.002~5.000 ng/L。将建立的方法应用于北京部分自备井水、市政末梢水和地表水样品的分析,结果在自备井水样中检出26种药物。

关键词: 超高效液相色谱-电喷雾串联质谱法, 代谢物, 固相萃取, 生活饮用水, 药物

Abstract:

A method for the determination of 54 drugs in drinking water samples was developed by using ultra-high performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-ESI MS/MS). The target drugs in drinking water samples were enriched and cleaned-up by HLB solid-phase extraction (SPE) cartridges and then eluted with 5 mL methanol. The elute was collected, concentrated under a gentle stream of nitrogen gas, diluted with 0.4 mL 0.1% formic acid solution, and analyzed by UPLC-ESI MS/MS. The separation of the 54 drugs was performed on an ACQUITY UPLCTMBEH C18 column using mobile phases of 0.1% formic acid and methanol by gradient elution. The multiple reaction monitoring (MRM) mode was employed in mass spectrometry acquisition. The matrix-matched external standard calibration was used for quantitation. The results showed that the average recoveries of the drugs in ground water, tap water and surface water were 58.7%-104.4%, 53.1%-109.5%, and 50.7%-118.8%, respectively, and the corresponding relative standard deviations (RSD, n=6) were 0.3%-12.8%, 1.0%-15.5%, and 0.4%-19.3%, respectively. The method quantification limits (MQL) for target compounds were in the range of 0.002-5.000 ng/L. The developed method was applied to analyze the water samples from Beijing. The results showed that 26 drugs were detected in ground water samples.

Key words: drinking water, drugs, metabolites, solid-phase extraction (SPE), ultra-high performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-ESI MS/MS)

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