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超高效液相色谱-串联质谱法同时测定环境水样中的15种抗生素

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崔敬鑫, 石秋俊, 王国民, 唐柏彬, 邱德生, 魏世强, 张进忠. 超高效液相色谱-串联质谱法同时测定环境水样中的15种抗生素[J]. 环境化学, 2020, (4): 1065-1074. doi: 10.7524/j.issn.0254-6108.2019042902
引用本文: 崔敬鑫, 石秋俊, 王国民, 唐柏彬, 邱德生, 魏世强, 张进忠. 超高效液相色谱-串联质谱法同时测定环境水样中的15种抗生素[J]. 环境化学, 2020, (4): 1065-1074. doi: 10.7524/j.issn.0254-6108.2019042902
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CUI Jingxin, SHI Qiujun, WANG Guomin, TANG Bobin, QIU Desheng, WEI Shiqiang, ZHANG Jinzhong. Simultaneous determination of 15 antibiotics in environmental water samples by ultra performance liquid chromatography- tandem mass spectrometry[J]. Environmental Chemistry, 2020, (4): 1065-1074. doi: 10.7524/j.issn.0254-6108.2019042902
Citation: CUI Jingxin, SHI Qiujun, WANG Guomin, TANG Bobin, QIU Desheng, WEI Shiqiang, ZHANG Jinzhong. Simultaneous determination of 15 antibiotics in environmental water samples by ultra performance liquid chromatography- tandem mass spectrometry[J]. Environmental Chemistry, 2020, (4): 1065-1074. doi: 10.7524/j.issn.0254-6108.2019042902
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超高效液相色谱-串联质谱法同时测定环境水样中的15种抗生素

  • 1. 西南大学资源环境学院, 重庆市农业资源与环境重点实验室, 重庆, 400715;

  • 2. 重庆海关技术中心, 重庆, 400020;

  • 3. 营山县环境监测站, 南充, 637700

    • 通讯作者: 张进忠, E-mail: jzhzhang@swu.edu.cn
  • 基金项目:

    重庆市技术创新与应用示范专项重点研发项目（cstc2018jszx-zdyfxmX0002）和国家重点研发计划项目（2018YFD0800601）资助.

Simultaneous determination of 15 antibiotics in environmental water samples by ultra performance liquid chromatography- tandem mass spectrometry

  • 1. College of Resources and Environment, Southwest University, Chongqing Key Laboratory of Agricultural Resources and Environment, Chongqing, 400715, China;

  • 2. Technical Center, Chongqing Customs, Chongqing, 400020, China;

  • 3. Environmental Monitoring Station of Yingshan County, Nanchong, 637700, China

    • Corresponding author: ZHANG Jinzhong, jzhzhang@swu.edu.cn
  • Fund Project: Supported by Chongqing Key Research & Development Program of Technology Innovation and Application Demonstration (cstc2018jszx-zdyfxmX0002) and the National Key Research & Development Program of China (2018YFD0800601).

  • 摘要: 采用固相萃取/超高效液相色谱-串联质谱法，建立了水样中磺胺类、四环素类、氟喹诺酮类、大环内酯类和氯霉素类15种抗生素的同时测定方法.水样经HLB固相萃取柱富集，ACQUITY UPLC BEH C18色谱柱分离，以乙腈和5 mmol·L-1乙酸铵溶液（含0.1%甲酸）为流动相梯度洗脱，电喷雾离子源-串联质谱多反应监测模式检测.结果表明，同时测定15种抗生素的线性范围为5-100 μg·L-1（相关系数均大于0.997），检出限为2.1-22.0 ng·L-1，定量限为6.9-71.8 ng·L-1；空白水样在加标水平为5、10、20 μg·L-1时，抗生素的回收率为50.1%-109.0%，相对标准偏差为0.4%-8.5%（n=7）.用本文建立的方法检测某农业小流域环境水样，发现5类抗生素可被不同程度检出，浓度范围为0.1-106.2 ng·L-1.
    Abstract: A simultaneous determination method for 15 antibiotics including sulfonamides, tetracyclines, quinolones, macrolides and chloramphenicols in water samples was developed by ultra performance liquid chromatography-tandem mass spectrometry with solid-phase extraction. The antibiotics in water samples were enriched by HLB solid-phase extraction column, and separated by ACQUITY UPLC BEH C18 column and eluted by acetonitrile and 5 mmol·L-1 ammonium acetate solution containing 0.1% formic acid as the mobile phases with gradient elution, and then determined by electrospray ion source-tandem mass spectrometry with multi-reaction monitoring mode. The results showed that the linear ranges were 5—100 μg·L-1 (R ≥ 0.997) with the detection limits of 2.1—22.0 ng·L-1 and the limits of quantification of 6.9—71.8 ng·L-1 for the simultaneous determination of 15 antibiotics. The recoveries of blank water sample spiked with 5, 10 and 20 μg·L-1 antibiotic standards were in the range of 50.1%—109.0% (0.4%≤RSDs≤8.5%, n=7). The five kinds of antibiotics in environmental water samples of an agricultural watershed could be detected with the range of 0.1—106.2 ng·L-1 by using the developed method in this study.
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  • 收稿日期:  2019-04-29

超高效液相色谱-串联质谱法同时测定环境水样中的15种抗生素

    通讯作者: 张进忠, E-mail: jzhzhang@swu.edu.cn
  • 1. 西南大学资源环境学院, 重庆市农业资源与环境重点实验室, 重庆, 400715;
  • 2. 重庆海关技术中心, 重庆, 400020;
  • 3. 营山县环境监测站, 南充, 637700
  • 收稿日期:  2019-04-29
基金项目:

重庆市技术创新与应用示范专项重点研发项目（cstc2018jszx-zdyfxmX0002）和国家重点研发计划项目（2018YFD0800601）资助.

摘要: 采用固相萃取/超高效液相色谱-串联质谱法，建立了水样中磺胺类、四环素类、氟喹诺酮类、大环内酯类和氯霉素类15种抗生素的同时测定方法.水样经HLB固相萃取柱富集，ACQUITY UPLC BEH C18色谱柱分离，以乙腈和5 mmol·L-1乙酸铵溶液（含0.1%甲酸）为流动相梯度洗脱，电喷雾离子源-串联质谱多反应监测模式检测.结果表明，同时测定15种抗生素的线性范围为5-100 μg·L-1（相关系数均大于0.997），检出限为2.1-22.0 ng·L-1，定量限为6.9-71.8 ng·L-1；空白水样在加标水平为5、10、20 μg·L-1时，抗生素的回收率为50.1%-109.0%，相对标准偏差为0.4%-8.5%（n=7）.用本文建立的方法检测某农业小流域环境水样，发现5类抗生素可被不同程度检出，浓度范围为0.1-106.2 ng·L-1.

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