[目的]建立超高效液相色谱-串联质谱同时测定羊肉中33种兽药残留的方法.[方法]样品用90%乙腈水(含2.0%甲酸)提取,通过Oasis Prime HLB净化,浓缩后用流动相定容.采用Waters ACQUITY UPLC HSS T3 柱(2.1 mm×100 mm,1.8 μm)分离.以甲醇和0.1%甲酸水为流动相梯度洗脱,在电喷雾离子源下正、负离子切换扫描,多反应监测(MRM)模式下,结合保留时间和特征离子信息,利用同位素内标法定量.[结果]33种兽药在0.5～40.0 ng/mL线性关系良好(r>0.99),最低检出浓度在0.08～0.10 ng/mL.加标回收率为83.7%～115.0%,RSD为0.58%～11.49%.[结论]该方法具有处理简单、灵敏度高、重复性好等优点,满足羊肉中33种兽药的定量检测.
Determination of 33 Veterinary Drug Residues in Mutton by Ultra High Performance Liquid Chromatography-Tandem Mass Spec-trometry with Isotope Internal Standard Method
[Objective]To establish a method for the simultaneous determination of 33 kinds of veterinary drug residues in mutton by ultra high performance liquid chromatography-tandem mass spectrometry.[Method]The sample was extracted with 90%acetonitrile water(containing 2.0%formic acid),purified by Oasis Prime HLB,concentrated,and diluted with mobile phase.Then separated by Waters ACQUITY UPLC HSS T3 column(2.1 mm×100 mm,1.8 μm),using 0.1%formic acid and acetonitrile as mobile phase.Under electrospray ionization source,switching between positive and negative ion modes,in Multiple Reaction Monitoring(MRM)mode,utilizing the isotope internal standard method for quantification by combining retention time and characteristic ion information.[Result]The linear relationship of the 33 kinds of veterinary drugs was good in the concentration range of 0.5-40.0 ng/mL(r>0.99),and the lowest detection concentration was 0.08-0.10 ng/mL.Adding standard recovery rates was 83.7%-115.0%,the RSD was 0.58%-11.49%.[Conclusion]The method has the simple processing,high sensitivty and good reproducibility,and is suitable for the quantitative detection of 33 kinds of veterinary drug residues in mutton.
UPLC-MS/MSIsotope internal standardMuttonVeterinary drug residues
万方数据
维普
