HPLC-MS/MS法研究恩诺沙星在鸡蛋中残留消除规律  

Investigation of Residues and Elimination Regularity of Enrofloxacin in Chicken Eggs by using HPLC-MS/MS

作　　者：侯轩 周炜 陈勇 张航俊 郭炫君 张晓丽 周芷锦 HOU Xuan;ZHOU Wei;CHEN Yong;ZHANG Hang-jun;GUO Xuan-jun;ZHANG Xiao-li;ZHOU Zhi-jin(Zhejiang Animal Disease Prevention and Control Center,Hangzhou 310020,China)

机构地区：[1]浙江省动物疫病预防控制中心,浙江杭州310020

出　　处：《畜牧与饲料科学》2020年第5期46-51,共6页Animal Husbandry and Feed Science

基　　金：浙江省科技厅重点研发计划项目“新型兽药研制及耐药性控制技术研发——动物源细菌耐药性监测与控制技术研究开发”(2019C02G4011294)。

摘　　要：建立了高效液相色谱—串联质谱法(HPLC-MS/MS)检测鸡蛋中恩诺沙星、环丙沙星残留的方法。鸡蛋样品经1%乙酸乙腈提取、正己烷除脂,用HPLC-MS/MS进行检测。恩诺沙星、环丙沙星在0.5~500 ng/mL浓度时线性关系良好(r≥0.999);恩诺沙星回收率为87.7%~99.1%、环丙沙星的回收率为89.1%~101.4%,检测限为0.5μg/kg,定量限为1.0μg/kg。应用该方法初步研究了恩诺沙星及其代谢物环丙沙星在鸡蛋中的残留消除规律。结果表明,给药后鸡蛋中恩诺沙星及其代谢物蓄积迅速,停药8 d后痕量恩诺沙星代谢缓慢,25 d后恩诺沙星代谢完全。A method for determination of enrofloxacin and ciprofloxacin residues in chicken eggs was developed using high-performance liquid chromatography coupled with tandem mass spectrometry(HPLC-MS/MS).After extraction by 1%acetic acid in acetonitrile and purified by hexane,the samples were analyzed by the established HPLC-MS/MS method.The calibration curves of enrofloxacin and ciprofloxacin were linear in the range of 0.5-500 ng/mL(r≥0.999);the recoveries of enrofloxacin in chicken eggs ranged from 87.7%to 99.1%,and those of ciprofloxacin in the samples ranged from 89.1%to 101.4%;the limit of detection and the limit of quantification of the established HPLC-MS/MS method for enrofloxacin and ciprofloxacin were 0.5μg/kg and 1.0μg/kg,respectively.The residues and elimination regularity of enrofloxacin and its metabolite ciprofloxacin in chicken eggs were preliminarily revealed by using a HPLC-MS/MS based method:the enrofloxacin and its metabolite were accumulated rapidly in eggs after the chicken were administrated,the metabolism of trace enrofloxacin was slow after 8 days of drug discontinuation,and the metabolism of enrofloxacin was complete after 25 days of drug discontinuation.

关 键 词：恩诺沙星 环丙沙星 鸡蛋 高效液相色谱—串联质谱法 

分 类 号：S859.84[农业科学—临床兽医学] O657.63[农业科学—兽医学]