快速检测畜禽肉中四环素等133种兽药残留  

Rapid detection method of tetracycline,etc. 133 veterinary drug residues in livestock and poultry meat

作　　者：梁君妮 曹鹏 张禧庆 李春蕾[3] 王文雯 胡巧茹 李晓玉 姜向柯 尹大路 

机构地区：[1]烟台出入境检验检疫局,烟台264000 [2]烟台杰科检测服务有限公司,莱阳265231 [3]烟台市动物疫病预防与控制中心,烟台264003

出　　处：《分析试验室》2017年第12期1411-1422,共12页Chinese Journal of Analysis Laboratory

基　　金：山东出入境检验检疫局科研项目(SK201612);国家质检总局科研项目(2015IK201)资助

摘　　要：建立了畜禽肉中133种兽药残留的快速检测方法,在避免使用缓冲盐的情况下实现了四环素与其他兽药的同时分析。样品经乙腈-水(4:1,V/V)提取,乙腈饱和正己烷和C18净化,适当氮吹浓缩后定容,再经乙腈饱和正己烷净化并高速离心,过0.22μm PTFE滤膜,LC-MS/M S分析。采用ACQUITYUPLC HSS T3色谱柱,梯度洗脱分离,电喷雾离子源(ESI),动态多重反应监测(Dynamic MRM)扫描。133种兽药在各自线性范围内,线性关系良好(r^2>0.99),定量限在0.05~50μg/kg之间。该方法适合于畜禽肉中多兽药残留的快速检测和定量。A method was developed for the rapid detection of 133 veterinary drugs residues in livestockand poultry meat. The method can analyze tetracycline and other veterinary drug residues at the same time, in the case to avoid using the buffer salt. The sample was extracted with acetonitrile-water（4：1, V/V）, purified by acetonitrile-saturated hexane and C18, concentrated by nitrogen blowing. Then solution was purified again by acetonitrile-saturated hexane and high speed centrifugation, and filtered through a 0. 22μm PTFE filter membrane. The drugs were separated on ACQUITYUPLC HSS 33 column by gradient elution, and analyzed by ultra-performance liquid chromatograohy-tandem mass spectrometry （UHPLC-MS/MS） in electrospray ionization （ESI） under dynamic multiple reaction monitoring （DynamicMRM） mode. All 133 drugs had good linearity in their respective linear ranges （ r2 〉 0. 99）, and the limits of quantification （LOQ） were 0. 05 - 50 lxg/kg, The method is a high- throughput detection method which can meet the requirement of domestic and international limited quantity, and is suitable for rapid detection and quantification of multi-veterinary drug residue in meat product.

关 键 词：多兽药残留 四环素 畜禽肉 快速检测 

分 类 号：O658[理学—分析化学]