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猪场废水中24种抗生素同时检测方法优化

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柴玉峰, 冯玉启, 张玉秀, 陈梅雪, 王瑞, 柳蒙蒙, 魏源送. 猪场废水中24种抗生素同时检测方法优化[J]. 环境化学, 2017, 36(10): 2147-2154. doi: 10.7524/j.issn.0254-6108.2017022301
引用本文: 柴玉峰, 冯玉启, 张玉秀, 陈梅雪, 王瑞, 柳蒙蒙, 魏源送. 猪场废水中24种抗生素同时检测方法优化[J]. 环境化学, 2017, 36(10): 2147-2154. doi: 10.7524/j.issn.0254-6108.2017022301
shu
CHAI Yufeng, FENG Yuqi, ZHANG Yuxiu, CHEN Meixue, WANG Rui, LIU Mengmeng, WEI Yuansong. Optimization of an analytical method for the simultaneous determination of 24 antibiotics in swine wastewater[J]. Environmental Chemistry, 2017, 36(10): 2147-2154. doi: 10.7524/j.issn.0254-6108.2017022301
Citation: CHAI Yufeng, FENG Yuqi, ZHANG Yuxiu, CHEN Meixue, WANG Rui, LIU Mengmeng, WEI Yuansong. Optimization of an analytical method for the simultaneous determination of 24 antibiotics in swine wastewater[J]. Environmental Chemistry, 2017, 36(10): 2147-2154. doi: 10.7524/j.issn.0254-6108.2017022301
shu

猪场废水中24种抗生素同时检测方法优化

  • 1.

    中国矿业大学(北京)化学与环境工程学院, 北京, 100083;

  • 2.

    北京建筑大学环境与能源工程学院, 北京, 100044;

  • 3.

    中国科学院生态环境研究中心, 北京, 100085

  • 基金项目:

    国家自然科学基金（41501513，21577161），中央高校基本科研业务费专项（2010YH05），国家科技重大专项参与单位任务（2015ZX07203-007-003）和国家重点研发计划课题（2016YFD0501405）资助.

Optimization of an analytical method for the simultaneous determination of 24 antibiotics in swine wastewater

  • 1.

    School of Chemical & Environmental Engineering, China University of Mining and Technology, Beijing, 100083, China;

  • 2.

    School of Energy & Environmental Engineering, Beijing University of Civil Engineering and Architecture, Beijing, 100044, China;

  • 3.

    Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing, 100085, China

  • Fund Project: Supported by the the State Natural Sciences Foundation(41501513,21577161),the Fundamental Research Funds for the Central Universities(2010YH05),National Science and Technology Major Project(2015ZX07203-007-003)and National Key Research and Invention Program(2016YFD0501405).

  • 摘要: 采用优化固相萃取-液相色谱-串联质谱同步检测养猪废水中24种抗生素的.水样用1 molL-1盐酸调节pH值至3.5-4.0，流经Oasis HLB固相萃取柱富集后再用甲醇和乙酸乙酯（V：V=1：1）进行洗脱.以Agilent eclipse plus C18色谱柱为分离柱，以0.1%甲酸水溶液和乙腈为流动相进行梯度洗脱，采用电喷雾正离子源，多反应监测模式检测.24种抗生素的检出限（S/N=3）在0.03-3.00 gL-1之间.进一步以不同养猪场废水进行实际样品测定，四环素类、大环内酯类、-内酰胺类、喹诺酮类、磺胺类等5大类抗生素均有检出，土霉素、替米考星和磺胺甲嘧啶等3种抗生素为主要污染抗生素，最高浓度可达147.10、107.83、100.20 gL-1，磺胺甲噻二唑及去甲基金霉素均未检出.本研究建立了快速准确的同步分析5大类24种抗生素的分析方法.
    Abstract: An optimized method employing solid phase extraction-liquid chromatography-tandem mass spectrometry was established for the simultaneous determination of 24 antibiotics in swine wastewater. After adjusting pH to 3.5-4.0 by using 1 molL-1 hydrochloric acid, the samples were concentrated and collected after flowing through an Oasis HLB solid-phase extraction column, and were eluted with methanol and ethyl acetate (V:V=1:1). The gradient elution was carried out with 0.1% (V:V) formic acid solution and acetonitrile as the mobile phase by using the Agilent eclipse plus C18 column, and the detection was performed under the monitoring mode of the electrospray ionization source multiple reaction. The limit of detection (S/N=3) of the 24 antibiotics was between 0.03-3.00 gL-1. Tetracyclines, macrolides, -lactams, quinolones and sulfonamides were all detected by this method in the swine wastewater samples. As the three main antibiotics, oxytetracycline, tilmicosin and sulfamethoxazole were found to have a maximum concentration of 147.10, 107.83 and 100.20 gL-1, respectively whereas sulfadoxadiazole and dimethyl chlortetracycline were not detected. The rapid and accurate detection of 24 antibiotics in 5 major classes was established.
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  • [1] ZHANG T, LI B. Occurrence, transformation, and fate of antibiotics in municipal wastewater treatment plants[J]. Critical Reviews in Environmental Science and Technology, 2011, 11(41):951-998.
    [2] [2] ZHAO L, DONG Y H, WANG H. Residues of veterinary antibiotics in manures from feedlot livestock in eight provinces of China[J]. Science of the Total Environment, 2010, 408(5):1069-1075.
    [3] [3] MANZETTI S, GHISI R. The environmental release and fate of antibiotics[J]. Marine Pollution Bulletin, 2014, 79(1-2):7-15.
    [4] [4] CHEE-SANFORD J C, MACKIE R I, KOIKE S, et al. Fate and transport of antibiotic residues and antibiotic resistance genes following land application of manure waste[J]. Journal of Environment Quality, 2009, 38(3):1086-1108.
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    [7] [11] CHEN H, LIU S, XU X, et al. Antibiotics in the coastal environment of the Hailing Bay region, South China Sea:Spatial distribution, source analysis and ecological risks[J]. Marine Pollution Bulletin, 2015, 95(1):365-373.
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    [9] [13] DI'AZ-CRUZ M S, LÍPEZ DE ALDA M J, BARCELÍ D. Environmental behavior and analysis of veterinary and human drugs in soils, sediments and sludge[J]. TrAC Trends in Analytical Chemistry, 2003, 22(6):340-351.
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    [11] [15] NAGESWARA RAO R, VENKATESWARLU N, NARSIMHA R. Determination of antibiotics in aquatic environment by solid-phase extraction followed by liquid chromatography-electrospray ionization mass spectrometry[J]. Journal of Chromatography A, 2008, 1187(1-2):151-164.
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出版历程
  • 收稿日期:  2017-02-23
  • 刊出日期:  2017-10-15
柴玉峰, 冯玉启, 张玉秀, 陈梅雪, 王瑞, 柳蒙蒙, 魏源送. 猪场废水中24种抗生素同时检测方法优化[J]. 环境化学, 2017, 36(10): 2147-2154. doi: 10.7524/j.issn.0254-6108.2017022301
引用本文: 柴玉峰, 冯玉启, 张玉秀, 陈梅雪, 王瑞, 柳蒙蒙, 魏源送. 猪场废水中24种抗生素同时检测方法优化[J]. 环境化学, 2017, 36(10): 2147-2154. doi: 10.7524/j.issn.0254-6108.2017022301
shu
CHAI Yufeng, FENG Yuqi, ZHANG Yuxiu, CHEN Meixue, WANG Rui, LIU Mengmeng, WEI Yuansong. Optimization of an analytical method for the simultaneous determination of 24 antibiotics in swine wastewater[J]. Environmental Chemistry, 2017, 36(10): 2147-2154. doi: 10.7524/j.issn.0254-6108.2017022301
Citation: CHAI Yufeng, FENG Yuqi, ZHANG Yuxiu, CHEN Meixue, WANG Rui, LIU Mengmeng, WEI Yuansong. Optimization of an analytical method for the simultaneous determination of 24 antibiotics in swine wastewater[J]. Environmental Chemistry, 2017, 36(10): 2147-2154. doi: 10.7524/j.issn.0254-6108.2017022301
shu

猪场废水中24种抗生素同时检测方法优化

  • 1.  中国矿业大学(北京)化学与环境工程学院, 北京, 100083;
  • 2.  北京建筑大学环境与能源工程学院, 北京, 100044;
  • 3.  中国科学院生态环境研究中心, 北京, 100085
  • 收稿日期:  2017-02-23
基金项目:

国家自然科学基金（41501513，21577161），中央高校基本科研业务费专项（2010YH05），国家科技重大专项参与单位任务（2015ZX07203-007-003）和国家重点研发计划课题（2016YFD0501405）资助.

摘要: 采用优化固相萃取-液相色谱-串联质谱同步检测养猪废水中24种抗生素的.水样用1 molL-1盐酸调节pH值至3.5-4.0，流经Oasis HLB固相萃取柱富集后再用甲醇和乙酸乙酯（V：V=1：1）进行洗脱.以Agilent eclipse plus C18色谱柱为分离柱，以0.1%甲酸水溶液和乙腈为流动相进行梯度洗脱，采用电喷雾正离子源，多反应监测模式检测.24种抗生素的检出限（S/N=3）在0.03-3.00 gL-1之间.进一步以不同养猪场废水进行实际样品测定，四环素类、大环内酯类、-内酰胺类、喹诺酮类、磺胺类等5大类抗生素均有检出，土霉素、替米考星和磺胺甲嘧啶等3种抗生素为主要污染抗生素，最高浓度可达147.10、107.83、100.20 gL-1，磺胺甲噻二唑及去甲基金霉素均未检出.本研究建立了快速准确的同步分析5大类24种抗生素的分析方法.

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