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

作　　者：余胜兵[1] 郑惠东[2] 鲁琳[1] 曲亚斌[1] 苏广宁[1] 林思仁[2] 朱杰民[1] 钟秀华[1] 黄伟雄[1] 朱炳辉[1] YU Shengbing1;ZHENG Huidong2;LU Lin 1;QU Yabin1;SU Guangning1;LIN Siren2;ZHU Jiemin;ZHONG Xiuhua1;HUANG Weixiong1;ZHU Binghui1

机构地区：[1]广东省疾病预防控制中心 [2]惠州市疾病预防控制中心

出　　处：《环境卫生学杂志》2018年第3期261-269,共9页JOURNAL OF ENVIRONMENTAL HYGIENE

基　　金：广东省医学科学技术研究基金项目(A2015061);惠州市科技计划项目(2015Y126)

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Na_2EDTA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(R^2>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。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（ R^2） 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 of58. 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.

关 键 词：抗生素 超高效液相色谱-串联质谱 固相萃取 饮用水 

分 类 号：R123[医药卫生—环境卫生学]