色谱 ›› 2016, Vol. 34 ›› Issue (3): 299-305.DOI: 10.3724/SP.J.1123.2015.10028

• 研究论文 • 上一篇    下一篇

高效液相色谱-质谱联用法同时检测水体中13种β-内酰胺类药物残留

朱峰, 吉文亮, 阮丽萍, 刘华良, 李放   

  1. 江苏省疾病预防控制中心, 江苏 南京 210009
  • 收稿日期:2015-10-18 出版日期:2016-03-08 发布日期:2012-09-28
  • 通讯作者: 李放
  • 基金资助:

    江苏科技厅科技支撑计划项目(BE2010745);江苏省"十二·五"科教兴卫工程项目(ZX201109).

Simultaneous determination of 13 β-lactam residues in water by high performance liquid chromatography-tandem mass spectrometry

ZHU Feng, JI Wenliang, RUAN Liping, LIU Hualiang, LI Fang   

  1. Jiangsu Provincial Center for Disease Prevention and Control, Nanjing 210009, China
  • Received:2015-10-18 Online:2016-03-08 Published:2012-09-28
  • Supported by:

    Jiangsu Science and Technology Department of Science and Technology Support Program (No. BE2010745); Key Provincial Talents Program in the 12th Five-Year Plan of Jiangsu Province (No. ZX201109).

摘要:

建立了一种利用高效液相色谱-质谱联用技术快速筛查检测水体中13种 β-内酰胺类药物残留的方法。水样经高速离心后过0.22 μm微孔滤膜直接进样,以0.05%甲酸水溶液和甲醇-乙腈(4 : 6, v/v)混合溶液为流动相进行梯度洗脱,经Atlantis dC-C18柱(150 mm×4.6 mm, 5 μm, Waters公司)分离,采用电喷雾离子源正离子电离、多反应监测模式检测。13种 β-内酰胺类化合物在线性范围内的线性关系均良好,相关系数(r2)均大于0.99,回收率均在81.4%~102.3%范围内,相对标准偏差均小于11%(n=7),检出限均在1.5~10 ng/L范围内。该方法快速、简便、灵敏,重现性好,为开展水体中抗生素污染水平的调查与监测提供了技术支持。

关键词: -内酰胺药物残留, &beta, 高效液相色谱-质谱联用, 抗生素, 水体

Abstract:

A rapid method for the simultaneous screening and determination of 13 β-lactam residues in water was developed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). After high speed centrifugation, the sample was filtered through a 0.22 μm microporous filter membrane, and then separated on an Atlantis dC-C18 column (150 mm×4.6 mm, 5 μm, Waters) with the gradient elution of water (containing 0.05% (v/v) formic acid) and methanol-acetonitrile (4 : 6, v/v). The electrospray ionization (ESI) source in positive ion mode was used for multiple reaction monitoring (MRM) mode. The 13 β-lactam chemical components showed good linear relationships in their concentration ranges with the correlation coefficients (r2) more than 0.99. The recoveries were all in the range of 81.4%-102.3%, and the relative standard deviations (RSDs) were all less than 11%(n=7). The limits of detection (LODs) were in the range of 1.5-10 ng/L. This method is rapid, simple, sensitive, accurate, and provides the basis for the investigation and monitoring of the pollution levels of the antibiotics in water.

Key words: β-lactam residues, antibiotics, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), water

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