高效液相色谱法和高效液相色谱-串联质谱法测定饲料中的甲苯咪唑及其代谢物残留量  

Dtermination of mebendazole and its metabolites in feed by HPLC and UPLC-MS/MS

作　　者：索纹纹[1,2] 李小玲 刘伶俐[1,2] 杨霄 万译文[1,2] SUO Wenwen;LI Xiaoling;LIU Lingli;YANG Xiao;WANG Yiwen(Hunan Fisheries Science Institute,Chang sha,Hunan province 410153,China;Fishery Products Quality Supervision and Testing Center,Ministry of Agriculture and Rural Affairs,Chang sha,Hunan province 410153,China)

机构地区：[1]湖南省水产科学研究所,湖南长沙410153 [2]农业农村部渔业产品质量监督检验测试中心(长沙),湖南长沙410153

出　　处：《中国饲料》2023年第16期61-64,共4页China Feed

摘　　要：建立了一种高效测定饲料中甲苯咪唑及其代谢物残留量的高效液相色谱法(HPLC)和高效液相色谱-串联质谱法(HPLC-MC/MS)分析方法。样品采用5%(V/V)甲酸化乙腈提取,提取液经EMR-Lipid dSPE柱去脂、EMR polish粉吸附净化,在40℃下用氮气吹至近干,采用乙腈-磷酸二氢铵(20:80,V/V)溶液复溶,过0.45μm尼龙滤膜后用HPLC法测定,或采用20%乙腈水溶液复溶后,过0.22μm尼龙滤膜后用HPLC-MS/MS法测定。甲苯咪唑及其代谢物的回收率为77.8%~112.1%,相对标准偏差为3.09%~7.28%。该方法具有比较高的重现性和选择性,在饲料中甲苯咪唑及其代谢物的残留测定中具有很好的应用前景。A high efficiency analysis method was established for the determination of mebendazole and its metabolites residue in feed by liquid chromatography and liquid chromatography-tandem mass spectrometry.The extracts,extracted with acetonitrile containing 5%(V/V)formic acid aqueous solution from samples,were defatted with EMR-Lipid dSPE column,and purified followed by clean up with EMR polish powder and dried 40℃under nitrogen flow.Finally,the extracts were redissolved in 2 mL(20:80,V/V)hydrophosphate aqueous solution and acetonitrile,filtered through 0.45μm membrane,and analyzed using UPLC,or redissolved in 1 mL 20%(V/V)acetonitrile and water solution,filtered through 0.22μm membrane,and detected using UPLC-MS/MS.The mean recovery the ratios of mebendazol and its metabolites ranged from 77.8%to 112.1%and the RSD ranged from 3.09%to 7.28%.The method proposed by this paper possesses higher prodicibility and selectivity,It is promising in real applications of determining the mebendazole and its metabolites residues in feeds.

关 键 词：甲苯咪唑 氨基甲苯咪唑 羟基甲苯咪唑 高效液相色谱 高效液相色谱-串联质谱法 饲料 

分 类 号：S816.17[农业科学—饲料科学]