色谱 ›› 2019, Vol. 37 ›› Issue (5): 525-532.DOI: 10.3724/SP.J.1123.2018.11016

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法同时测定表层水体中5类40种抗生素

封梦娟1,2, 杨正标3, 张芹2, 宋宁慧2, 刘艳华1, 郭瑞昕1, 陈建秋1, 张圣虎2   

  1. 1. 中国药科大学工学院, 江苏 南京 211198;
    2. 生态环境部南京环境科学研究所, 江苏 南京 210042;
    3. 南京市环境监测中心站, 江苏 南京 210013
  • 收稿日期:2018-11-11 出版日期:2019-05-08 发布日期:2015-03-23
  • 通讯作者: 陈建秋,E-mail:cjqalga@163.com;张圣虎,E-mail:zsh@nies.org
  • 基金资助:

    国家自然科学基金(21876207,21507165,21407055).

Simultaneous determination of five types of 40 antibiotics in surface water using high performance liquid chromatography-tandem mass spectrometry

FENG Mengjuan1,2, YANG Zhengbiao3, ZHANG Qin2, SONG Ninghui2, LIU Yanhua1, GUO Ruixin1, CHEN Jianqiu1, ZHANG Shenghu2   

  1. 1. School of Engineering, China Pharmaceutical University, Nanjing 211198, China;
    2. Nanjing Institute of Environmental Sciences, Ministry of Ecology and Environment, Nanjing 210042, China;
    3. Nanjing Environmental Monitoring Center Station, Nanjing 210013, China
  • Received:2018-11-11 Online:2019-05-08 Published:2015-03-23
  • Supported by:

    National Natural Science Foundation of China (Nos. 21876207, 21507165, 21407055).

摘要:

建立了固相萃取-高效液相色谱-串联质谱(SPE-HPLC-MS/MS)同时检测表层水中5类40种抗生素的分析方法。水样经过滤、固相萃取柱富集净化后,以乙腈-0.2%(v/v)甲酸水溶液为流动相进行梯度洗脱,采用电喷雾电离源,在多反应监测、正离子模式进行定性定量分析。结果显示,40种抗生素在1~200 μg/L水平下线性关系良好,平均加标回收率为41.3%~112.6%。采用该方法对长江南京段表层水体进行检测,共检出13种抗生素,含量为13.4~780.5 ng/L,其中喹诺酮类抗生素恩诺沙星检出率达100%,大环内酯类抗生素克林霉素最高检出水平达739.4 ng/L。该法高效、灵敏、可靠,可用于实际水样中多种抗生素的分析。

关键词: 表层水, 高效液相色谱-串联质谱, 固相萃取, 抗生素

Abstract:

A method was developed for the determination of five categories of 40 antibiotics in surface water by using solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry (SPE-HPLC-MS/MS). The water samples were enriched and cleaned-up by filtration and with SPE cartridges. All antibiotics were separated by gradient elution with the mobile phase of 0.2% (v/v) formic acid aqueous solution and acetonitrile, and then analyzed with an electrospray ionization source in the positive ion and multiple reaction monitoring (MRM) modes. The results showed that the 40 antibiotics achieved great linearity in the range of 1-200 μg/L, and the average recoveries ranged from 41.3% to 112.6%. Using the developed method, thirteen antibiotics were identified in surface water from Nanjing section of the Yangtze River. The total antibiotic contents in the real samples ranged from 13.4 ng/L to 780.5 ng/L. The established method is efficient, sensitive and reliable, and is suitable for the determination of different antibiotics in real water samples.

Key words: antibiotics, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), solid phase extraction (SPE), surface water

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