色谱

色谱 ›› 2015, Vol. 33 ›› Issue (4): 348-353.DOI: 10.3724/SP.J.1123.2014.09028

• 研究论文 • 上一篇    下一篇

固相萃取-高效液相色谱-串联质谱法同时测定养殖海水中23种抗生素

杜鹃, 赵洪霞, 陈景文   

  1. 工业生态与环境工程教育部重点实验室, 大连理工大学环境学院, 辽宁 大连 116024
  • 收稿日期:2014-11-18 修回日期:2014-10-29 出版日期:2015-04-08 发布日期:2015-03-30
  • 通讯作者: 陈景文
  • 基金资助:

    国家重点基础研究计划("973")课题(2013CB430403).

Simultaneous determination of 23 antibiotics in mariculture water using solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry

DU Juan, ZHAO Hongxia, CHEN Jingwen   

  1. Key Laboratory of Industrial Ecology and Environmental Engineering of Ministry of Education, Department of Environmental Science and Technology, Dalian University of Technology, Dalian 116024, China
  • Received:2014-11-18 Revised:2014-10-29 Online:2015-04-08 Published:2015-03-30

PDF

276

被引次数

28

摘要：

建立了固相萃取-高效液相色谱-串联质谱(SPE-HPLC-MS/MS)同时检测水中6类23种抗生素的分析方法。水样用固相萃取柱富集净化,通过对比水样在不同上样pH、洗脱液用量等条件下的回收率,优化了前处理方法。采用0.1%(v/v)甲酸-1 g/L甲酸铵水溶液和甲醇-乙腈(1:1, v/v)体系作为流动相,经过梯度洗脱进行分离,在HPLC-MS/MS多反应监测模式下进行定性定量分析。结果显示,23种抗生素的方法检出限(MDL)范围为0.1~2.9 ng/L,加标回收率为47.3%~132.6%。采用该方法对东营海水养殖区5个养殖池水样进行了检测,除青霉素类之外的各类抗生素均有检出,其中磺胺增效剂甲氧苄氨嘧啶的检出率达100%,氯霉素类抗生素氟甲砜霉素检出的最高质量浓度达到261.0 ng/L。结果表明,所建立的方法高效、灵敏、可靠,可用于海水中多种抗生素的分析。

关键词: 高效液相色谱-串联质谱, 固相萃取, 抗生素, 养殖海水

Abstract:

A method for the determination of 23 antibiotics from 6 categories in water was developed by using solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry (SPE-HPLC-MS/MS). Water samples were enriched and cleaned-up by solid-phase extraction cartridges. The MS detection parameters of the analyzed antibiotics, the pH values of loading buffers and the volumes of the eluents were optimized by comparing the sample recoveries under different conditions. All antibiotics were separated by gradient elution with the mobile phases of 0.1% (v/v) formic acid and 1 g/L ammonium formate in water and acetonitrile-methanol (1:1, v/v) mixture. The eluate was then analyzed by HPLC-MS/MS in both positive and negative electrospray ionization conditions with multiple reaction monitoring (MRM) mode. The method detection limits (MDLs) were in the range of 0.1-2.9 ng/L and the recoveries of 23 antibiotics in water ranged from 47.3% to 132.6%. The developed method was applied to the analysis of 5 water samples from mariculture ponds located in Dongying City, Shandong Province. The results showed that the antibiotics could be detected in all water samples. The trimethoprim showed the highest detection rate, and the florfenicol had the highest mass concentration which reached 261.0 ng/L. The results showed that the developed method is efficient, sensitive and reliable, which is suitable for the detection of antibiotics in seawater samples.

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

中图分类号: