高效液相色谱法测定动物性食品中4种β2-兴奋剂.pdfVIP

中国卫生检验杂志2008年7月第18卷第7期 Chinese Jounaal of Health Laboratory Technology，Jul 2008；Vol 18 No 7 1227 【论著】 高效液相色谱法测定动物性食品中4种l32一兴奋剂 王炼 ，黎源倩 (1．四川大学华西公共卫生学院，成都 610041；2．成都市疾病预防控制中心，成都 610041) [摘要] 目的：建立动物性食品中4种B 一兴奋剂：奥西那林、克伦特罗、沙丁胺醇和非诺特罗的高效液相色谱一二级 管阵列检测的方法。方法：动物组织样品用缓冲溶液匀浆后，酶水解，高氯酸沉淀蛋白后，滤液调至碱性，用乙酸乙酯：异 丙醇(6：4)提取后，旋转蒸发去除溶剂。缓冲液溶解后，过C 一SCX串联固相萃取小柱，甲醇淋洗后分析，对于含蛋白、 脂肪少的动物食品样品，酶解并沉淀蛋白，滤液调至pH3后过C 一SCX串联固相萃取小柱，洗脱液用于分析。结果：对 含蛋白、脂肪少的样品，样品加标回收率在60．6％～88．0％，精密度在2．72％～7．86％；含蛋白、脂肪多的样品，加标回收 率在60．1％～84．9％，精密度在1．26％～6．20％，方法在0．2～50．0 ml有良好线性。样品的最低检出浓度：奥西那 林为0．07 mg／kg；沙丁胺醇为0．10 mg／kg；非诺特罗为0．08 mg／ ；克伦特罗为0．04 mg／kg。结论：本方法操作简便、准 确灵敏、重现性好、分析成本较低。 [关键词] 动物性食品；高效液相色谱法；串联固相萃取；酶水解；B：一兴奋剂 [中图分类号] 0657．7 2 [文献标识码] A [文章编号] 1004—8685(2008)07—1227—04 Determination of four I；2一agonists in animal food by high performance liquid chromatog。 raphy Wang Lian ．Li Yuan—qian (1．College of Huaxi Public Health，Sichuan University，Chengdu 610041，China；2．Chengdu Center for Disease Control and Pre— vention，Chengdu 610041，China) [Abstract] Objective：In this study，a enzymatic hydrolyzation—C18一SCX(Strong Cation Ion Exchange)tandem SPE—high performance liquid chromatography—PAD method for four B2一agonists in animal food was developed and evaluated．Methods： Homogenized in buffer solution and hydrolyzed by enzyme，sample tissue with much protein was deposited with HC104，centri— fuged，and extracted with additional organic solution at adjusted alkaline pH which was evaporated revolvely later．The residue was dissolved in salt，transited by SCX—C18 tandem SPE and analysed after washed by aminated methano1．On the other hand，after hydrolyzed by enzyme，sample tissue with little protein was centrifuged at p