色谱

色谱 ›› 2016, Vol. 34 ›› Issue (2): 176-183.DOI: 10.3724/SP.J.1123.2015.09021

• 研究论文 • 上一篇    下一篇

固相萃取-超高效液相色谱-串联质谱法测定畜禽饮用水中23种抗生素和3种β-受体激动剂

石奥   

  1. 北京市畜牧业环境监测站, 北京 102200
  • 收稿日期:2015-09-18 出版日期:2016-02-08 发布日期:2012-09-11
  • 通讯作者: 石奥
  • 基金资助:

    北京市农委基金项目(PXM2014 036240 000012).

Determination of 23 antibiotics and 3 β-agonists in livestock drinking water by ultra performance liquid chromatography-tandem mass spectrometry coupled with solid-phase extraction

SHI Ao   

  1. Beijing Monitoring Station for Animal Husbandry Environment, Beijing 102200, China
  • Received:2015-09-18 Online:2016-02-08 Published:2012-09-11
  • Supported by:

    Beijing Municipal Agricultural Commission Fund (Grant No. PXM2014 036240 000012).

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摘要：

建立了固相萃取-超高效液相色谱-串联质谱同时测定畜禽饮用水中4类23种抗生素(磺胺类、喹诺酮类、四环素类、氯霉素类)和3种 β-受体激动剂(克伦特罗、莱克多巴胺、沙丁胺醇)的分析方法。样品经高氯酸调节pH至5.0,加入乙二胺四乙酸二钠(Na2EDTA), HLB固相萃取柱富集,用超高效液相色谱-质谱联用仪分时段多反应监测离子模式分析,外标法定量抗生素,内标法定量 β-受体激动剂。23种抗生素和3种 β-受体激动剂的空白基质加标回收率为50.7%~104.6%,相对标准偏差(n=3)为2.6%~8.8%。23种抗生素和3种 β-受体激动剂的线性关系良好,相关系数均大于0.994,检出限为0.01~0.20 ng/L。通过该方法分析了北京地区36家规模化畜禽养殖场畜禽饮用水中的抗生素和 β-受体激动剂,检出了多种抗生素,并对含量进行了定量计算。

关键词: β-受体激动剂, 超高效液相色谱-串联质谱, 固相萃取, 抗生素, 畜禽饮用水

Abstract:

A method has been developed for the simultaneous determination of 23 antibiotics (four categories) and 3 β-agonists in livestock drinking water using solid-phase extraction and ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC-ESI MS/MS). The samples were adjusted pH to 5.0, added Na2EDTA, enriched and cleaned-up by an HLB solid-phase extraction cartridge. The target compounds were confirmed and quantified by UPLC-ESI MS/MS with external standard method for the antibiotics and internal standard method for the β-agonists. The recoveries were assessed by using lab tap water as matrix. The average recoveries of the 23 antibiotics and the 3 β-agonists were in the range of 50.7%-104.6% and the relative standard deviations (RSDs) were 2.6%-8.8%(n=3). Under the optimal conditions, the calibration curves of the 23 antibiotics and the 3 β-agonists showed good linearity with the correlation coefficients better than 0.994. The limits of detection (LODs, S/N≥3) ranged from 0.01-0.20 ng/L. The developed method was applied to analyze the livestock drinking waters in 36 Beijing intensive livestock farms. The results showed that some antibiotics were detected.

Key words: β-agonists, antibiotics, livestock drinking water, solid-phase extraction, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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