色谱

色谱

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高效液相色谱-电喷雾串联质谱法检测环境水样中22种抗生素类药物

高立红1,2, 史亚利1, 厉文辉1, 刘杰民2, 蔡亚岐1*   

  1. 1. 中国科学院生态环境研究中心环境化学与生态毒理学国家重点实验室, 北京 100085; 2. 北京科技大学土木与环境工程学院, 北京 100083
  • 收稿日期:2010-01-14 修回日期:2010-02-14 出版日期:2010-05-28 发布日期:1980-09-25
  • 通讯作者: 蔡亚岐

Determination of 22 antibiotics in environmental water samples using high performance liquid chromatography-electrospray ionization tandem mass spectrometry

GAO Lihong1,2, SHI Yali1, LI Wenhui1, LIU Jiemin2, CAI Yaqi1*   

  1. 1. State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Science, Chinese Academy of Sciences, Beijing 100085, China; 2. Civil and Environment Engineering School, University of Science and Technology Beijing, Beijing 100083, China
  • Received:2010-01-14 Revised:2010-02-14 Online:2010-05-28 Published:1980-09-25
  • Contact: CAI Yaqi

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1445

被引次数

72

摘要： 建立了高效液相色谱-电喷雾串联质谱(HPLC-ESI MS/MS)分析环境水样中22种抗生素类药物的方法。采用HLB固相萃取柱对环境水样中的目标化合物进行富集、净化,然后以6 mL氨水-甲醇(5:95, v/v)溶液洗脱。收集的洗脱液经氮气吹干至1 mL,然后进行HPLC-ESI MS/MS分离分析。色谱流动相A相为甲醇-乙腈(1:1, v/v), B相为0.3%(体积分数)甲酸水溶液(含0.1%(体积分数)甲酸铵,pH 2.9);色谱柱为XTerra MS C18柱。质谱检测采用正离子扫描,多反应监测模式。分别以自来水和污水作为基质,22种抗生素类药物的加标平均回收率分别为54.9%～130%和57.4%～138%,相对标准偏差(n=3)分别为2.85%～28.6%和2.02%～23.2%;方法的检出限为0.05～0.5 ng/L。将建立的方法应用于北京市高碑店湖和小清河水样的分析,结果表明在两个水样中均有部分抗生素类药物检出。

关键词: 高效液相色谱-电喷雾串联质谱法, 固相萃取, 环境水样 , 抗生素类药物

Abstract: A method for the determination of 22 antibiotics in environmental water samples was developed by using high performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI MS/MS). The target antibiotics in water samples were enriched and cleaned-up by HLB solid-phase extraction (SPE) cartridges, and then eluted with 6 mL ammonium hydroxide-methanol (5:95, v/v). The eluate was collected and concentrated to 1 mL under a gentle stream of nitrogen gas, and then analyzed by HPLC-ESI MS/MS in positive electrospray ionization and multiple reaction monitoring (MRM) mode. The separation was carried out on an XTerra MS C18 column with mobile phases of A, methanol-acetonitrile (1:1, v/v), and B, 0.3% formic acid/water (containing 0.1% ammonium formate, v/v, pH 2.9). The results showed that the average recoveries of antibiotics in tap water and wastewater were 54.9%~130% and 57.4%~138%, respectively, and the corresponding relative standard deviations (RSD, n=3) were 2.85%~28.6% and 2.02%~23.2%, respectively. The method detection limits were 0.05~0.5 ng/L. The developed method was applied to analyze the water samples of Gaobeidian Lake and Xiaoqinghe River in Beijing. The results showed that some antibiotics were detected both in the two samples.

Key words: antibiotics, environmental water samples , solid-phase extraction(SPE), high performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI MS/MS)