液相色谱串联质谱分析肉鸡毛发中诺氟沙星残留  

Analysis of norfloxacin residues in broiler hair by LC-MS/MS

作　　者：向建军 袁丽娟[1] 廖且根[1] 张大文[1] 罗林广[1] 扎西次旦 XIANG Jianjun;YUAN Lijuan;LIAO Qiegen;ZHANG Dawen;LUO Linguang;ZHAXI Cidan(Agricultural Product Quality Safety and Standards Institute,Jiangxi Academy of Agricultural Sciences,Nanchang 330200;Institute of Agricultural Quality Standards and Testing,Tibet Academy of Agricultural and Animal Husbandry Sciences,Lhasa 850000)

机构地区：[1]江西省农业科学院农产品质量安全与标准研究所,南昌330200 [2]西藏农牧科学院农业质量标准与检测研究所,拉萨850000

出　　处：《分析试验室》2020年第5期556-559,共4页Chinese Journal of Analysis Laboratory

基　　金：江西省现代农业科研协同创新专项(JXXTCX201602-06);西藏农牧厅科技项目(XZ201801NB09)资助。

摘　　要：建立了一种适用于肉鸡毛发中诺氟沙星残留分析的方法。毛发样品经医用纱布包裹后清洗,剪碎后加入4 mol/L氨水超声提取,Oasis HLB修饰磁纳米材料用于净化提取液,采用Agilent Eclipse Plus C18色谱柱分离,电喷雾正离子源进行离子化,多反应监测方式(MRM)对诺氟沙星的母离子及子离子进行监测,三重四极杆质谱测定。该方法鸡毛中诺氟沙星在1. 0~100. 0$g/kg范围线性良好,相关系数为0. 9928;诺氟沙星检出限为0. 3$g/kg,定量限为1. 0$g/kg,方法回收率为89. 2%~95. 7%;相对标准偏差(RSDs)均小于10%。方法可满足政府和企业在肉鸡饲养期间对诺氟沙星的监控需求。A method for the identification and quantification of norfloxacin residue in broiler hair samples by LCMS/MS was developed. Hair samples were cleaned after being wrapped in gauze,then sheared and added to4 mol/L ammonia solution for ultrasonic extraction. The extract was purified by Oasis HLB modified magnetic nanomaterials. The samples were analyzed by LC-MS/MS. The LC separation was performed on an Agilent Eclipse Plus C18 column. Multiple reaction monitoring( MRM) was used for the selective detection of norfloxacin. The good linearity curve of norfloxacin was in the range from 1. 0 to 100. 0 $g/kg with correlation coefficient of 0. 9928. And the limit detection and limit of quantification were 0. 5 and 1. 0 $g/kg in spiked hair samples,respectively. The recoveries of norfloxacin were 89. 2 %-95. 7%,and the relative standard deviations( RSDs) were less than 10%. The established method could meet the need of government and enterprises to monitor the illegal use of norfloxacin during the whole rearing period.

关 键 词：诺氟沙星 鸡毛 检测 液相色谱串联质谱 

分 类 号：O657.63[理学—分析化学] S8-05[理学—化学]