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液相色谱-电喷雾串联质谱法对废水中喹诺酮和氟喹诺酮类抗生素的痕量分析

Trace analysis of quinolone and fluoroquinolone antibiotics from wastewaters by liquid chromatography-electrospray tandem mass spectrometry.

作者信息

Xiao Yang, Chang Hong, Jia Ai, Hu Jianying

机构信息

College of Urban and Environmental Sciences, Peking University, Beijing 100871, China.

出版信息

J Chromatogr A. 2008 Dec 19;1214(1-2):100-8. doi: 10.1016/j.chroma.2008.10.090. Epub 2008 Oct 31.

Abstract

A sensitive liquid chromatography-electrospray tandem mass spectrometry method, combined with solid-phase extraction and a weak cation exchange cartridge cleanup, was established for twenty quinolone and fluoroquinolone antibiotics (pipemidic acid, flerofloxacin, ofloxacin, pefloxacin, enoxacin, norfloxacin, ciprofloxacin, danofloxacin, enrofloxacin, lomefloxacin, difloxacin, sarafloxacin, gatifloxacin, sparfloxacin, moxifloxacin, cinoxacin, oxolinic acid, nalidixic acid, flumequine, and piromidic acid) in influent, effluent, and river waters. For the various water matrices considered, the overall recoveries were from 64% to 127% except for piromidic acid (27-33%), and no obvious matrix effect was observed. The method detection limits for the twenty target antibiotics in the influent, effluent, and surface water samples were 1.6-50 ng/L, 0.6-50 ng/L, and 0.8-50 ng/L, respectively. This method was applied to analyze residual quinolone and fluoroquinolone antibiotics in wastewater and surface water samples from Beijing, China. Eight antibiotics (12 (pipemidic acid)-1208 ng/L (ofloxacin)) were detected in wastewater, and seven (1.3 (lomefloxacin)-535 ng/L (ofloxacin)) were detected in surface water samples. Gatifloxacin, a 4th generation fluoroquinolone antibiotic, was detected for the first time in influent (111 ng/L), effluent (56 ng/L), and river water (16-42 ng/L).

摘要

建立了一种灵敏的液相色谱 - 电喷雾串联质谱法,结合固相萃取和弱阳离子交换柱净化,用于测定进水、出水和河水中的20种喹诺酮类和氟喹诺酮类抗生素(吡哌酸、氟罗沙星、氧氟沙星、培氟沙星、依诺沙星、诺氟沙星、环丙沙星、达氟沙星、恩诺沙星、洛美沙星、二氟沙星、沙拉沙星、加替沙星、司帕沙星、莫西沙星、西诺沙星、恶喹酸、萘啶酸、氟甲喹和吡咯米酸)。对于所考虑的各种水基质,除吡咯米酸(27 - 33%)外,总体回收率为64%至127%,未观察到明显的基质效应。进水、出水和地表水样品中20种目标抗生素的方法检出限分别为1.6 - 50 ng/L、0.6 - 50 ng/L和0.8 - 50 ng/L。该方法应用于分析中国北京废水和地表水样品中残留的喹诺酮类和氟喹诺酮类抗生素。废水中检测到8种抗生素(12(吡哌酸) - 1208 ng/L(氧氟沙星)),地表水中检测到7种(1.3(洛美沙星) - 535 ng/L(氧氟沙星))。首次在进水(111 ng/L)、出水(56 ng/L)和河水中(16 - 42 ng/L)检测到第四代氟喹诺酮类抗生素加替沙星。

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