建立了采用Oasis PriMEHLB固相萃取柱净化-超高效液相色谱-串联质谱法同时测定生鲜乳中45种兽药残留含量的方法。该法为样品经质量分数为0.2%甲酸乙腈沉淀蛋白后,通过Oasis PriME HLB固相萃取柱一次性净化除去磷脂及非极性干扰物;用Waters HSS T3色谱柱,流动相为0.1%甲酸水(质量分数10%甲醇)-乙腈(含10%甲醇)梯度洗脱,电喷雾-正离子多反应监测模式(除氯霉素),内标法定量。该方法在质量浓度为1-50ng/mL范围内线性良好,45种兽残相关系数r均大于0.991。经添加1,5,10μg/kg三个质量分数水平的加标样品的测定,回收率在62.1%-118%之间,RSD%在1.5-9.4之间,方法的准确性和重复性良好。
a method for the simultaneous determination of 45 kinds of veterinary drug residues in fresh milk by PriME HLB Oasis solid phase extraction column purification-ultra high performance liquid chromatography tandem mass spectrometry was established. The method for the sample with 0.2% formic acid acetonitrile protein precipitation, the oasis PriME HLB solid-phase extraction column disposablecleaning to remove phospholipids and non polarity disruptors; waters HSS T3 column. The mobile phase was 0.1% formic acid in water (containing 10% methanol) -acetonitrile (containing 10% methanol gradient elution and electrospray ionization in positive ion multiple reaction monitoring mode (except chloramphenicol), internal standard quantitative method. The method was linear in the range of 1-50 ng/mL, and the cor- relation coefficient between the 45 species and the residual correlation coefficient r was more than 0.991. With the addition of 1 g/kg, 5 g/kg, 10 g/kg three concentration levels, the recovery rate was between 118% and 62.1%, and the accuracy and repeatability of the method was between 9.4 and 1.5.