固相萃取-气相色谱质谱测定动物组织中氯霉素的残留量  

Determination of Chloramphenicol Residue in Animal Tissues by Solid Phase Extraction and Gas Chromatography-Mass Spectrometry

作　　者：谢孟峡[1] 刘媛[1] 邱月明[1] 韩杰[1] 刘宜孜[1] 

机构地区：[1]北京师范大学分析测试中心,北京100875

出　　处：《分析化学》2005年第1期1-4,共4页Chinese Journal of Analytical Chemistry

基　　金：国家科技攻关计划食品安全重大专项基金资助项目(No. 2001BA804A18)

摘　　要：对鸡肉、猪肉、猪肝、鸭肝等动物组织样品中的氯霉素残留的检测方法进行了研究.用乙酸乙酯和磷酸盐缓冲溶液提取动物组织中的氯霉素残留,用硅胶和C18固相萃取柱对乙酸乙酯提取物进行净化和富集.净化后的提取物用BSTFA衍生化和气相色谱-质谱-负化学电离源选择离子定量检测(选择离子为376,378,466,468,470).通过对提取、净化富集条件的优化,建立了动物组织中氯霉素残留量的检测方法. 该方法对不同基体样品的加标回收率为80%～100%之间;相对标准偏差小于20%;方法的检出限为0.1μg/kg.Determination method of chloramphenicol residue in animal tissues ( chicken, pork, liver of pig and liver of duck) was investigated. Acetate ester and phosphate buffer were used to extract the chloramphe nicol residue in animal tissues.' The acetate ester extracts were further purified and enriched by silica and C,, solid phase extraction cartridges. The final extracts were derivatised with N, O-bis ( trimetylsilyl) trifluooroacetamide (BSTFA) and chloramphenicol was quantitatively determined by gas chromatography-mass spectrometry with negative chemical ionization source in selected ion mode ( ions selected was 376, 378, 466, 468, 470). The extraction and purification conditions were optimized. The recoveries of this method for fortified samples in different matrix are between 80% similar to 100%, and the relative standard deviations are below 20%. The limit of detection of the method is below 0.1 mug/kg.

关 键 词：动物组织 乙酸乙酯提取物 氯霉素残留量 定量检测 质谱测定 残留量 检测方法 鸡肉 猪肉 样品 

分 类 号：TS251.7[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]