摘要
建立了环境水体中15种喹诺酮类抗生素和6种雌激素的HPLC-MS/MS分析方法。该方法统一了两类物质的前处理过程,运用固相萃取技术进行富集及净化,有效降低了基质的干扰。质谱采用SRM监测模式,喹诺酮采用正离子扫描模式,雌激素采用负离子扫描模式。目标化合物在水体中的回收率范围为62.0%～108.3%,RSD在1.1%～9.2%之间。雌酮、雌二醇、雌三醇的方法检出限均为0.30ng/L;己烷雌酚、己烯雌酚、炔雌醇的方法检出限均为0.14ng/L;氟甲喹、诺氟沙星、依诺沙星、洛美沙星、沙拉沙星检出限为0.90 ng/L;氟罗沙星、氧氟沙星、环丙沙星、恩诺沙星、单诺沙星、奥比沙星、双氟沙星、司帕沙星、麻保沙星、噁喹酸检出限为0.50 ng/L。方法适用于水体中雌激素和喹诺酮类抗生素的分析和监测。
A method for simultaneous determination of 15 quinolone antibiotics and 6 estrogens in environmental water samples was developed by high performance liquid chromatography tandem mass spectrometry in this work.A unified pretreatment method was established for the two groups of compounds.The samples were extracted and cleaned up by using solid-phase extraction（SPE） instrument with HLB cartridge.Using SPE method,the matrix effect was minimized efficiently.The positive ion scan mode of mass spectrometry was used for quinolones and negative ions for estrogens,and the SRM transition was taken.The recoveries of the target compounds in water samples ranged from 62.0% to 108.3% and the relative standard deviations（RSD） ranged from 1.1% to 9.2%.Determination limits were 0.30 ng/L for E1,E2 and E3;0.14ng/L for HEX,HES and EE2;0.90ng/L for OA,NOR,ENO,LOM and SAR;FLE,OFL,CIP,ENR,DAN,ORB,DIF,SPR,MAR and FLU.This method has been successfully applied to the survey of estrogens and quinolone antibiotic residues in environmental water samples.
出处
《分析试验室》
CAS
CSCD
北大核心
2011年第12期8-12,共5页
Chinese Journal of Analysis Laboratory
基金
国家海洋局青年科学基金项目(20090507)
海洋公益性项目(201105013)资助
