同位素作内标气质联机测定动物源食品中4种β2-兴奋剂的含量.pdfVIP

2194 中国卫生检验杂志2007年l2月第l7卷第l2期 Chinese Journal of Health Laboratory Technology，Dec 2007；Vol 17 No 12 【化学测定方法】 同位素作内标气质联机测定动物源食品中4种132一兴奋剂的含量 管健 ，王立媛 ，吴平谷 ，曹家穗 ，朱国英 ，葛淼华 (1．浙江省嘉兴市疾病预防控制中心，浙江嘉兴 314050； 2．浙江省绍兴市疾病预防控制中心，浙江绍兴 312041；3．浙江省疾病预防控制中心，杭州 310009) [摘要] 目的：建立用同位素作内标，GC／MS测定动物源食品中4种B2一兴奋剂含量的分析方法。方法：粉碎的样品中 添加内标加高氯酸匀浆，用高氯酸沉淀蛋白质，正己烷脱脂，再经阳离子交换柱子(SLS)净化，再用N，O双(三甲基硅基) 三氟乙酰胺一三甲基氯硅烷(BSTFA+TMCS，99+1)衍生化，用同位素作内标，同时测定4种p2一兴奋剂。结果：4种p2 一 兴奋剂对肝、肾和肉样品进行添加回收实验，平均回收率为70％～130％(n：6)，变异系数为4％～16％(n：6)。结 论：本方法准确性好、灵敏度高、简便、快速，为动物源食品中B2一兴奋剂的检测提供了可参考的分析方法。 [关键词] B2一兴奋剂；同位素；气相色谱一质谱 [中图分类号] 0657．63 [文献标识码] A [文章编号] 10O4—8685(2007)12—2194—03 Study on determination of 4 一agonistic residues in foods from animal source with iso- topically labelld internal standard by GC／MS Guan Jian’ Wang Li—yll,ctn ，Wu P ng—gu ，Cao Jia—sui ，Zhu Guo—ying ， Miao—hua ， (1．Jiaxing Center for Disease Control and Prevention，Jiaxing 314050，China；2．Shaoxing Centerfor Disease Control and Preven— tion，Shaoxing 312041，China；3．Zh~iang Center for Disease Control and Prevention，Hangzhou 310009，China) [Abstract] 0bjective：To establish a practical method for the simultaneous determination of Clenbuterol，Ractopamine，Salbu— tamo1．Terbutaline residues in foods from animal source with isotopically labelld internal standard by Gas chromatograph—mass spectrometry(GC／MS)．Methods：Sample spiked with isotopically labelld internal standard was homogenized with perchloricacid， the protein was precipitated with perchloricacid，followed by defatted with hexane．Further cleanup was performed on a SLS car- tridge．The purified 4 132一agonists and the isotope were derivatized with[N，O—bis(trimethylsily1)trifluoroaeetamide(BSTFA) 一 trimethylchlorosilane(TMCS)，99+1]，internal standard and 4 132一agonists were determined at one time．