固相萃取-高效液相色谱/串联质谱同时检测动物源性食品中76种兽药残留  

Simultaneous Determination of 76 Veterinary Drug Residues in Foodstuffs of Animal Origin by Solid Phase Extraction-Liquid Chromatography-Tandem Mass Spectrometry

作　　者：郭德华[1] 邓晓军[1] 赵善贞[1] 朱坚[1] 夏崇菲[2] 陈舜胜[2] 宋越[3] 

机构地区：[1]上海出入境检验检疫局,上海200135 [2]上海海洋大学,上海200433 [3]中国药科大学,南京211198

出　　处：《分析化学》2010年第3期318-324,共7页Chinese Journal of Analytical Chemistry

基　　金：上海市科委技术标准专项(No.08DZ0505200);上海出入境检验检疫局科技专项(No.HK004-2007)资助

摘　　要：建立了固相萃取-高效液相色谱/串联质谱(SPE-HPLC/MS)同时测定动物源性食品中76种兽药残留的检测方法。样品采用乙腈和含Mg2+的柠檬酸缓冲液进行提取,去除有机相后以缓冲液重溶,聚合物和阳离子交换固相萃取柱串联净化,用甲醇和甲醇-氨水(95∶5,V/V)分步洗脱,液相色谱-串联质谱进行测定,基质曲线外标法定量。方法的定量下限为0.5μg/kg(β-受体激动剂类和三苯甲烷类)、1.0μg/kg(苯二氮卓类和硝基咪唑类)、5.0μg/kg(苯并咪唑类)和20μg/kg(磺胺类)。76种兽药在虾、猪肉、猪肝、鸡蛋和牛奶中的基质溶液标准曲线线性相关系数(r)大于0.907,回收率在59.4%～115.3%之间,相对标准偏差在2.6%～27.3%之间。采用本方法对市场中样品进行筛选,发现2例阳性样品中含有莱克多巴胺和地西泮残留,测定值分别为0.92和6.5μg/kg。A method based on solid phase extraction-liquid chromatography-tandem mass spectrometry for the simultaneous determination of 76 veterinary drugs in foodstuffs of animal origin was presented. The residues derived from pork,shrimp,milk,liver and egg were extracted by acetonitrile combined with citrate buffer containing magnesium cation. The extracts were distilled and redissolved with citrate buffer followed by a further cleanup procedure using polymer connected with cation exchange SPE column. The residues retained in column were rinsed with methanol and mixture of methanol and ammonium hydroxide（ 95∶5,V/V） . Sample matrix-matched calibration was used to determine the residue contents by external standard. The method provided a LOQ of 0. 5 μg/kg （ β-agonist and triphenylmethane） ,1. 0 μg/kg （ benzodiazepine and nitroimdazole） ,5. 0 μg/kg（ benzimidazole） and 20. 0 μg/kg（ sulfanilamide） ,linear relationship more than 0. 907 and a recovery ranged from 59. 4% to 115. 3% with a RSD between 2. 6% and 27. 3% in sample matrix. The practical inspection using the method offered two positive samples for ractopamine and diazepam with a residual concentration of 0. 92 and 6. 5 μg/kg.

关 键 词：兽药 残留 高效液相色谱-串联质谱 动物源性产品 

分 类 号：TS207.5[轻工技术与工程—食品科学]