俞慧红


摘要[目的]建立一种简单、准确、快速而又重现性好的气相色谱-质谱联用法(GCMS)测定动物组织中盐酸克伦特罗的预处理方法。[方法]以猪肝为原料,预处理方法是样品在碱化的条件下用乙酸乙酯提取,用酸性水溶液反萃取,SCX固相萃取小柱净化,经双三甲基硅烷三氟乙酰胺(BTSFA)衍生后,再采用气质联用仪进行检测其盐酸克伦特罗的含量。[结果]研究显示,该方法下盐酸克伦特罗的回收率为85%~95%,检出限可达0.5 μg/kg。[结论]采用气相色谱-质谱联用法测定动物组织中盐酸克伦特罗的精密度高,重现性好,方法可靠。
关键词盐酸克伦特罗;动物组织;预处理;气相色谱-质谱联用法
中图分类号S851.34+7文献标识码A文章编号0517-6611(2016)04-130-03
Pretreatment of Clenbuterol Hydrochloride in Animal Tissue Detection by GCMS Method
YU HuiHong (Food and Drug Inspection and Testing Center of Cixi City,Cixi,Zhejiang 315300)
Abstract [Objective] To establish a simple,accurate,rapid and repeatable GCMS method,which was a pretreatment method to detect the clenbuterol hydrochloride in animal tissues.[Method] With pig liver as the raw material,extraction was carried out in alkaline condition by ethyl acetate.Acidic aqueous solution was used for backextraction.After purification by SCX solid phase extraction column,and derivation by doubletrimethylsilyl trifluoroacetamide (BTSFA),GCMS was used for detection.[Result] The recovery rate of clenbuterol hydrochloride was 85%95%; and detection limit reached 0.5 μg/kg.[Conclusion] Detecting clenbuterol hydrochloride in animal tissues by GCMS has high precision,good repeatability and reliable results.
Key wordsClenbuterol hydrochloride; Animal tissue; Pretreatment; GCMS
鹽酸克伦特罗(Clenbuterol,CLB),其化学名为羟甲叔丁肾上腺素或2[(叔丁氨基)甲基]4氨基3,5二氯苯甲醇盐酸盐,药品名为双氯醇胺、克喘素、氨哮素。它是强效选择性β2受体激动剂,有强而持久的松弛支气管平滑肌的作用,将其添加于饲料中,能促进家畜生长,减少酮体脂肪沉积,提高瘦肉率,故又称“瘦肉精”。但食用含盐酸克伦特罗较高的动物组织后,人体会出现肌肉颤动、肌痛、心动过速,甚至恶心、头晕目眩等中毒症状[1]。
目前,盐酸克伦特罗的检测方法已经比较成熟,我国现有的检测标准主要有国家标准GB/T 5009.192-2003《动物性食品中克伦特罗残留量的测定》[2]、农业部推荐性标准NY/T 468-2006《动物组织中盐酸克伦特罗的测定气相色谱/质谱法》[3],检测方法主要集中在酶免疫分析法、高效液相色谱法、气质联用仪法等。……