超高效液相色谱-串联质谱同时测定饮用水中60种抗生素

余胜兵; 郑惠东; 鲁琳; 曲亚斌; 苏广宁; 林思仁; 朱杰民; 钟秀华; 黄伟雄; 朱炳辉

doi:10.13421/j.cnki.hjwsxzz.2018.03.018

超高效液相色谱-串联质谱同时测定饮用水中60种抗生素

Simultaneous Determination of 60 Kinds of Antibiotics in Drinking Water Samples by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

摘要

摘要:
目的建立饮用水中60种抗生素同时测定的方法。
方法水样调节pH至2.0后，加入同位素内标和金属螯合剂Na₂EDTA充分混匀。用HLB固相萃取小柱进行富集净化浓缩，超高效液相色谱-串联质谱（UPLC-MS/MS）测定分析，内标法定量。
结果抗生素的检出限在（0.001~0.6）ng/L，定量限在（0.004~1.9）ng/L。大部分抗生素在（0.2~40）ng/L范围内，相关系数良好（R²>0.99）。低、中、高三种浓度抗生素水样的加标回收率在58.3%~127.7%。精密度（RSD）在1.6%~13.9%。采用所建立的方法对水源水、出厂水和管网末梢水进行分析，获得了满意的结果。
结论本文建立的方法具有操作简单、灵敏、快速、准确的优点，适用于饮用水中抗生素的多残留同时测定。

Abstract:
Objectives To establish a method for simultaneous determination of 60 kinds of antibiotics in water samples by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).
Methods After the pH value of water sample was adjusted to 2.0, the water sample was then concentrated and purified by an oasis HLB solid phase extraction column, analyzed by UPLC-MS/MS analysis and quantified by internal standard method.
Results A good linearity for the majority of antibiotics in water samples was in the range of (0.2~40) ng/L, with a correlation coefficient (R²) of ≥ 0.99, the limit of determination (LOD) was (0.001~0.6) ng/L and the limit of quantification (LOQ) was (0.004~1.9) ng/L.The spiked recovery of samples were in the range of 58.3%~127.7% at 3 spike levels (1, 4 and 20 ng/L).The relative standard deviations (RSDs) were in the range of 1.6%~13.9%.
Conclusions The established method was simple, rapid and accurate, which could be applied to the determination and quantification of the residue of antibiotics in water samples.

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