收稿日期院2016-09-13曰收到修改稿日期院2016-11-23 基金项目院国家 863 课题渊2013AA06A309冤曰苏州农业职业技术学院青年教师科研能力提升计划资助项目渊PPS201304冤 作者简介: 徐 洁渊1983-冤袁女袁江苏苏州市人袁讲师袁硕士袁主要从事环境保护研究遥 通信作者院鲜啟鸣渊1966-冤袁男,江苏金湖市人,教授,博士,主要从事新型有机污染物环境行为研究。 固相萃取-高效液相色谱-串联质谱测定水中 5 种大环内酯类抗生素 徐 洁 1 袁 邓 超 2 袁 鲜啟鸣 2 ( 1. 苏州农业职业技术学院环境工程学院,江苏苏州 215008; 2. 南京大学环境学院 污染控制与资源化研究国家重点实验室,江苏 南京 210023 ) 摘 要院建立固相萃取渊SPE冤尧高效液相色谱-串联质谱渊HPLC-MS/MS冤同时测定水中 5 种大环内酯类抗生素渊罗红霉 素尧克拉霉素尧阿奇霉素尧螺旋霉素和泰乐菌素冤的分析方法遥 水样中的抗生素通过 Oasis HLB 固相萃取小柱富集 后袁以 C18 反相色谱柱为分析柱袁甲醇和 0.1%甲酸水溶液为流动相袁采用 HPLC-MS/MS 进行定量分析袁检测方式为 多反应监测模式渊MRM冤袁内标法定量遥5 种大环内酯类抗生素的回收率在 64.8%耀90.8%之间袁仪器检出限为 0.012耀 0.085 滋g/L袁定量限为 0.041耀0.285 滋g/L遥 将建立的方法用于检测某化学工业园区周边地表水中 5 种目标分析物的残 留袁均未检测到泰乐菌素袁其余 4 种抗生素均有不同程度检出袁检出浓度在 ng/L 水平遥 关键词院大环内酯类抗生素曰固相萃取曰高效液相色谱-串联质谱曰水体 文献标志码院A 文章编号院1674-5124渊2017冤03-0058-05 Simultaneous determination of 5 macrolides antibiotics in natural water samples using solid phase extraction-high performance liquid chromatography-tandem mass spectrometry XU Jie 1 ,DENG Chao 2 ,XIAN Qiming 2 ( 1. School of Environmental Engineering, Suzhou Polytechnic Institute of Agriculture, Suzhou 215008, China; 2. State Key Laboratory of Pollution Control and Resource Reuse, School of Environment, Nanjing University, Nanjing 210023, China ) Abstract: A method with solid phase extraction ( SPE ) and high performance liquid chromatography- tandem mass spectrometry ( HPLC-MS/MS ) was developed for the determination of five macrolides ( roxithromycin, clarithromycin, azithromycin, spiramycin and tylosin ) in natural water samples. The macrolides were extracted from water samples using Oasis HLB cartridges and then separated on a reverse phase column using methanol and 0.1% formic acid as mobile phases. The macrolides were quantified with the internal standard method under multiple reaction monitoring ( MRM ) mode. The recoveries of the five macrolides ranged from 64.8% to 90.8% . The instrumental limits of detection and quantification are 0.012-0.085 滋g/L and 0.041-0.285 滋g/L respectively. Only Tylosin was not found by the proposed method in the studied rivers surrounding a Chemical Industry Park,while the other four macrolides were detected at the ng/L level. Keywords: macrolides antibiotics ( MLs ); solid phase extraction ( SPE ); high performance liquid chromatography-tandem mass spectrometry ( HPLC-MS/MS );water 中国测试 CHINA MEASUREMENT & TEST Vol.43 No.3 March, 2017 第 43 卷第 3 期 2017 年 3 月 doi院10.11857/j.issn.1674-5124.2017.03.012
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Simultaneous determination of 5 macrolides antibiotics in natural water samplesusing solid phase extraction-high performance liquid chromatography-tandem
mass spectrometry
XU Jie1,DENG Chao2,XIAN Qiming2
(1. School of Environmental Engineering,Suzhou Polytechnic Institute of Agriculture,Suzhou 215008,China;2. State Key Laboratory of Pollution Control and Resource Reuse,School of Environment,
Nanjing University,Nanjing 210023,China)
Abstract: A method with solid phase extraction(SPE)and high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) was developed for the determination of five macrolides(roxithromycin, clarithromycin, azithromycin, spiramycin and tylosin) in natural water samples.The macrolides were extracted from water samples using Oasis HLB cartridges and then separatedon a reverse phase column using methanol and 0.1% formic acid as mobile phases. The macrolideswere quantified with the internal standard method under multiple reaction monitoring(MRM)mode.The recoveries of the five macrolides ranged from 64.8% to 90.8% . The instrumental limits ofdetection and quantification are 0.012-0.085 滋g/L and 0.041-0.285 滋g/L respectively. Only Tylosinwas not found by the proposed method in the studied rivers surrounding a Chemical IndustryPark,while the other four macrolides were detected at the ng/L level.Keywords: macrolides antibiotics(MLs);solid phase extraction (SPE);high performance liquidchromatography-tandem mass spectrometry(HPLC-MS/MS);water
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