高效液相色谱-串联质谱法对水环境中12种抗生素的检测

doi:10.12066/j.issn.1007-2861.1655

上海大学学报(自然科学版) ›› 2017, Vol. 23 ›› Issue (3): 483-490.doi: 10.12066/j.issn.1007-2861.1655

• 研究论文 • 上一篇

高效液相色谱-串联质谱法对水环境中12种抗生素的检测

徐晖, 吴明红, 徐刚

上海大学环境与化学工程学院, 上海 200444

收稿日期:2015-03-30 出版日期:2017-06-30 发布日期:2017-06-30
通讯作者: 吴明红(1968—), 女, 教授, 博士生导师, 博士, 研究方向为污染控制与环境毒理学. E-mail: mhwu@staff.shu.edu.cn
作者简介:吴明红(1968—), 女, 教授, 博士生导师, 博士, 研究方向为污染控制与环境毒理学. E-mail: mhwu@staff.shu.edu.cn
基金资助:
国家自然科学基金资助项目(41430644, 11175112, 41373098, 41273141, 41473090)

Determination of 12 antibiotics in aqueous environment by high performance LC-MS/MS

XU Hui, WU Minghong, XU Gang

School of Environmental and Chemical Engineering, Shanghai University, Shanghai 200444, China

Received:2015-03-30 Online:2017-06-30 Published:2017-06-30

摘要/Abstract

摘要：

利用固相萃取(solid phase extraction, SPE)及液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry, LC-MS/MS)联用技术, 建立了水体中痕量磺胺类、β-内酰胺类、四环素类、喹诺酮类、大环内酯类等12 种抗生素的定量分析方法. 水样中的12 种抗生素通过亲水疏水平衡(hydrophile lipophilic balance, HLB)小柱的萃取富集后, 以乙腈为有机相、0.2% 甲酸和醋酸铵混合水溶液为水相, 采用LC-MS/MS 进行定量分析. 抗生素采用电喷雾电离(electrospray ionization, ESI)源多反应监测(multiple reaction monitoring, MRM)模式, 以¹³C3-caffeine 作为内标物进行定量检测. 抗生素在河水中的方法定量限为0.004 83~4.805 00 ng/L, 回收率为71%90%. 该方法被应用于分析南陈河(上海)中抗生素的含量, 平均质量浓度为2.04254.46 ng/L.

关键词: 样品前处理, 液相色谱-串联质谱, 抗生素

Abstract:

This paper proposes a quantitative method for trace detection of 12 antibiotics including sulfonamides, β-lactams, fluoroquinolones, tetracyclines, macrolides in waters using solid phase extraction (SPE) coupled to liquid chromatography-tandem mass spectrometry (LC-MS/MS). After enriching thought hydrophile lipophilic balance (HLB) cartridges, 12 antibiotics are detected by LC-MS/MS with the organic phase of acetonitrile and aqueous phase of ammonium acetate and 0.2% formic acid. The antibiotics are quantified with multiple reaction monitoring (MRM) mode by internal standard of ¹³C3-caffeine. Quantification limits for antibiotics are from 0.004 83 to 4.805 00 ng/L in river water and the recoveries ranged from 71% to 90%. The method is applied to detect antibiotics in Nanchen River, Shanghai. Mean concentrations of antibiotics are from 2.04 to 254.46 ng/L.

Key words: liquid chromatography-tandem mass spectrometry (LC-MS/MS), sample pretreatment, antibiotics

徐晖, 吴明红, 徐刚. 高效液相色谱-串联质谱法对水环境中12种抗生素的检测[J]. 上海大学学报(自然科学版), 2017, 23(3): 483-490.

XU Hui, WU Minghong, XU Gang. Determination of 12 antibiotics in aqueous environment by high performance LC-MS/MS[J]. Journal of Shanghai University（Natural Science Edition）, 2017, 23(3): 483-490.

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高效液相色谱-串联质谱法对水环境中12种抗生素的检测

Determination of 12 antibiotics in aqueous environment by high performance LC-MS/MS

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