水环境中磺胺类抗生素固相萃取-液质联用检测方法的建立及效果评估  

Establishment of solid phase extraction-liquid mass spectrometry method for detection of sulfa antibiotics in water environment and its effect evaluation

作　　者：范素素[1] 方烨渟 蔡萌 马艳 石健[1] FAN Susu;FANG Yeting;CAI Meng;MA Yan;SHI Jian(Analysis and Testing Center of Nantong University,Nantong 226019,China;School of Chemistry and Chemical Engineering,Nantong University,Nantong 226019,China)

机构地区：[1]南通大学分析测试中心,南通226019 [2]南通大学化学化工学院,南通226019

出　　处：《环境工程学报》2022年第8期2764-2774,共11页Chinese Journal of Environmental Engineering

基　　金：南通市社会民生科技计划(MS12020048);江苏省水利科技项目(2020043);江苏省大型科学仪器开放共享自主研究课题(TC2021A021)。

摘　　要：为快速、同步检测分析磺胺类抗生素,有效削减并控制水体中磺胺类上抗生素含量,基于已有检测仪器和分析测试方法,建立了一种用于同时测定水体中8种磺胺类抗生素(磺胺氯哒嗪、磺胺间二甲氧嘧啶、磺胺二甲基嘧啶、磺胺甲恶唑、磺胺喹恶啉、磺胺甲氧哒嗪、磺胺甲噻二唑、磺胺吡啶)残留的固相萃取-液相色谱-三重四极杆串联质谱检测方法;在检测过程中,调节水样的pH为3,用HLB固相萃取柱进行净化、富集,在40℃条件下用氮吹浓缩吹干,用超纯水复溶至1 mL;以0.1%甲酸水溶液和0.1%甲酸乙腈溶液作为流动相,使用Phenomenex Kinetex F5色谱柱(50 mm×3.0 mm,2.6μm)进行分离,在多反应监测模式(MRM)下对样品进行定量、定性分析。结果表明:8种磺胺类抗生素线性关系良好,且拟合度均大于0.9990;检出限为0.1~0.5μg·L^(−1),定量限为0.5~2.0μg·L^(−1);质量浓度为1、5、50μg·L^(−1)的混标溶液的加标回收率分别为78.85%~127.96%、76.69%~114.38%和73.55%~125.92%,相对标准偏差均在15%以内。该方法快捷、高效、灵敏,能够满足水中磺胺类抗生素的定性、定量检测,可为我国检测方法标准体系的建设提供参考。In order to quickly and synchronously detect and analyze sulphonamides,effectively reduce and control sulphonamides content in water,based on the existing detection instruments and analysis and testing methods,a liquid chromatography-triple quadrupole tandem mass spectrometry method was developed to simultaneously detect the residues of 8 antibiotics in water:sulfadiazine,sulfadimethyrimidine,sulfadimethyrimidine,sulfamethoxazole,sulfamequinoline,sulfamethoxyazine,sulfamethothiazole,sulfamepyridine.During the detecting process,the sulfonamides in water samples were enriched with HLB solid phase extraction column at pH=3,then dried by nitrogen blowing at 40℃and re-dissolved to 1mL by ultrapure water,lastly separated by Phenomenex Kinetex F5 column(50 mm×3.0 mm,2.6μm)using 0.1%formic acid aqueous solution and 0.1%formic acid acetonitrile as mobile phase.The results showed that there was a good linear relationship between the 8 sulfonamides antibiotics and the fitting degree was higher than 0.999.The limits of detection were 0.1~0.5μg·L^(−1),and the limits of quantification were 0.5~2.0μg·L^(−1).The recoveries of mixed standard solutions with mass concentrations of 1,5 and 50μg·L^(−1) were 78.85%~127.96%,76.69%~114.38%and 73.55%~125.92%,respectively,and the relative standard deviations(RSD)were not higher than 15%.The method is quick,efficient and sensitive,and can satisfy the qualitative and quantitative detection of sulfa antibiotics in water.It can provide a reference for the construction of standard system of detection methods in China.

关 键 词：磺胺类抗生素 固相萃取 液质联用 环境水体 残留检测 

分 类 号：X502[环境科学与工程—环境工程]