UPLC-MS/MS检测七种动物源食品中四环素类药物残留量的研究  

Optimized Determination of Tetracyclines in Seven Kinds of Animal Derived Food by UPLC / MS / MS

作　　者：张鑫[1] 吴剑平[1] 李丹妮[1] 严凤[1] 曹莹[1] 顾欣[1] 

机构地区：[1]上海市动物疫病预防控制中心,上海201103

出　　处：《中国兽药杂志》2015年第12期36-42,共7页Chinese Journal of Veterinary Drug

基　　金：上海市市级农口系统青年人才成长计划(沪农青字(2014)第2-5号);上海市科技兴农重点攻关项目(沪农科攻字(2013)第6-9号)

摘　　要：研究并优化了七种不同动物源食品中四环素、土霉素、金霉素、多西环素残留的超高效液相色谱-串联质谱检测方法。选用Na2EDTA-Mc Ilvaine缓冲溶液作为提取液,超声提取七种动物源食品中四环素类残留,C18固相萃取小柱净化,脱溶剂后用甲醇水溶解,在超高效液相色谱-串联质谱上进行检测。结果显示,猪肉、鸡肉、鸡蛋、鱼肉、牛奶中四环素类药物残留的最低定量限(LOQ)为10μg/kg,猪肾、猪肝最低定量限(LOQ)为20μg/kg,在定量限到2倍最大残留限量(MRL)的添加范围内,回收率为75%±25%,RSD<10%,可以满足农业部235号公告的要求。A UPLC / MS / MS method for determination of the residues of tetracyclines（ tetracycline,oxytetracycline,chlortetracycline and doxycycline） in seven different kinds of animal derived food was studied and optimized. The tetracyclines in seven kinds of animal derived food were pretreated with extraction by Na2EDTA-Mc Ilvaine buffer solution,purification by C18 SPE column,dissolution by CH3 OH / H2O（ 50 /50,V / V） after desolvation,and then determined by UPLC / MS / MS. The results showed that the recoveries were in the range of50% ～ 100% when blank samples spiked with tetracyclines in 10 μg / kg or 20 μg / kg ～ 2MRL,and the relative standard deviation was less than 10%. The method could satisfy the request of legislation on maximum residue limits in the ministry of agriculture 235 announcement.

关 键 词：兽药残留 四环素类 优化 超高效液相色谱-串联质谱 

分 类 号：S859.84[农业科学—临床兽医学]