超高效液相色谱-串联质谱法测定鲜蛋中喹诺酮类化合物  

Determination of Fluoroquinolones Residues in Fresh Eggs by UPLC-MS/MS

作　　者：陈玉威 孙晓娟 周子人 高广慧 CHEN Yuwei;SUN Xiaojuan;ZHOU Ziren;GAO Guanghui(Liaoning Inspection Examination and Certification Centre,Shenyang 110036,China)

机构地区：[1]辽宁省检验检测认证中心,辽宁沈阳110036

出　　处：《品牌与标准化》2024年第6期22-24,共3页

基　　金：辽宁省应用基础研究计划项目(2022JH2/101300076):食品安全非靶向筛查及溯源识别关键技术研究。

摘　　要：采用QuEChERS法进行前处理,建立超高效液相色谱-串联质谱同时测定鲜蛋中喹诺酮类化合物的检测方法,并对样品前处理和色谱条件进行优化。采用酸化乙腈提取样品,盐析,离心取上清液,40℃水浴下氮气吹干,复溶后用正己烷去除脂溶性杂质,取下层溶液过滤,用UPLC-MS/MS进行测定。结果表明,喹诺酮类化合物在2~100μg/L相关系数大于0.99,检出限和定量限分别为0.5μg/kg和2μg/kg,回收率在87.3%~109.1%,相对标准偏差为1.3%~10.2%(n=6),利用所建立的方法有7份样品检出恩诺沙星。本方法简单、经济、实用,适用于鲜蛋中的喹诺酮类化合物的测定。A method for the simultaneous determination of Fluoroquinolones in fresh eggs by UPLC-MS/MS was established using QuEChERS pretreatment,and the sample pretreatment and chromatographic conditions are optimized.The sample is extracted using acidified acetonitrile,salting out,centrifuged to obtain the supernatant,dried under nitrogen in a 40°C water bath,and after reconstitution,lipid soluble impurities were removed using n-hexane.The lower layer solution is filtered and analyzed using UPLC-MS/MS.The results shows that the correlation coefficient of fluoroquinolones between 2~100μg/L is greater than 0.99,with detection and quantification limits of 0.5 and 2μg/kg,respectively.The recovery rate is between 87.3%~109.1%,with a relative standard deviation of 1.3%~10.2%(n=6).Seven samples are detected for enrofloxacin using the established method.This method is simple,economical,and practical,suitable for the determination of quinolone compounds in fresh eggs.

关 键 词：超高效液相色谱-串联质谱法 鲜蛋 喹诺酮 检测 

分 类 号：O657.63[理学—分析化学] TS253.7[理学—化学]