动物性食品中阿维菌素类药物残留检测高效液相色谱法的优化  

Optimization of High Performance Liquid Chromatography for the Detection of Avermectins Residues in Animal Foods

作　　者：谭梅 李燕君 李然[2] 吴晓岚[2] 岳秀英[2] 吕晓华 TAN Mei;LI Yan-jun;LI Ran;WU Xiao-lan;YUE Xiu-ying;LYU Xiao-hua(West China School of Public Health and West China Fourth Hospital,Sichuan University,Chengdu 610041,China;Veterinary Drug Supervision of Sichuan Province,Chengdu 610041,China)

机构地区：[1]四川大学华西公共卫生学院华西第四医院,四川成都610041 [2]四川省兽药监察所,四川成都610041

出　　处：《中国兽医杂志》2019年第10期86-90,共5页Chinese Journal of Veterinary Medicine

基　　金：四川省科技计划(2019YFS0062);四川大学高校基本科研业务费研究专项项目(skqy201234)。

摘　　要：为探索方便快捷且符合兽药残留试验技术规范要求的阿维菌素类药物残留检测方法,对农业部1025号公告-5-2008动物性食品中阿维菌素类药物残留检测-酶联免疫吸附法、高效液相色谱法和液相色谱-串联质谱法中的高效液相色谱法进行优化,改进了样品提取后储存条件、净化条件和衍生化条件。牛肝样品经2次乙腈提取后,用乙腈-水-三乙胺储存备用,用C18固相萃取柱分离,1-甲基咪唑-乙腈、三氟乙酸酐-乙腈、冰乙酸和三乙胺衍生化,乙腈作流动相,高效液相色谱法分析。优化法试验结果显示,爱普菌素、阿维菌素、伊维菌素和多拉菌素等4种阿维菌素类药物在2~200μg/L的浓度范围内,标准曲线线性良好,相关系数均大于0.999 2;方法检测限2μg/kg,定量限5μg/kg;加标回收率在83%~93%,批内变异系数小于14%,批间变异系数小于11%。表明优化法符合兽药残留试验技术规范的要求,准确度和精密度较好,检测时间和成本低于标准法,可用于动物性食品中阿维菌素类药物残留的检测。To develop a convenient and rapid method for the determination of avermectins residues to meet the technical specifications of veterinary drug residue test,we optimized the High Performance Liquid Chromatography in the standard method of Ministry of Agriculture No.1025 Announcement-5-2008 Detection of avermectins in animal foods!Enzyme-Linked Immunosorbent Assay,and the High Performance Liquid Chromatography and Liquid Chromatography-Tandem Mass Spectrometry.The storage conditions,purification conditions and derivative conditions were improved.After two times of acetonitrile extraction,the beef liver samples were stored in acetonitrile-water-triethylamine,separated by C18SPE column,and derivated by 1-methyl imidazol-acetonitrile,trifluoroacetic anhydride-acetonitrile,glacial acetic acid and triethylamine.Acetonitrile was used as mobile phase for HPLC analysis.The experimental results of optimized methods showed that the standard carve of eprinomectin,avermectin,doramectin and ivermectin was linear carve between 2μg/L and 200μg/L.The correlation coefficients were greater than 0.9992.The detection limits and the quantitative limits of the 4 drugs were 2μg/kg and 5μg/kg.The recoveries determined were between 83%and 93%,and the coefficient of variations of intra and inter were less than 14%and 11%.The optimized method meets the technical specifications of veterinary drug residue test.It has good accuracy and precision.The detection time and cost are lower than the standard method.It can be used for the detection of avermectins residues in animal foods.

关 键 词：动物性食品 阿维菌素类药物 高效液相色谱法 优化 

分 类 号：S859.84[农业科学—临床兽医学]