| 摘要: |
| 本文了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。本方法选用Na2EDTA-McIlvaine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，经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?Ee25%，RSD<10%，可以满足农业部235号公告的要求。 |
| 关键词: 兽药残留 四环素类 超高效液相色谱-串联质谱 优化 |
| DOI： |
| 投稿时间：2015-10-27修订日期：2015-11-12 |
| 基金项目: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 |
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| Optimized Determination of Tetracyclines in Seven Kinds of Animal Derived Food by UPLC/MS/MS |
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| (Shanghai Animal Disease Control Center) |
| Abstract: |
| 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-McIlvaine buffer solution，purification by C18 SPE column, dissolution by CH3OH/H2O(50/50, v/v) after desolvation，and then determined by UPLC/MS/MS. The results showed that the recoveries were in the range of 50%~100% when blank samples spiked with tetracyclines in 10?g/kg or 20?g/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. |
| Key words: veterinary residue tetracyclines UPLC/MS/MS optimize |
