超快速液相–质谱法同时测定液体奶和奶粉中磺胺和喹诺酮类药物残留

建立超快速液相–质谱联用法测定乳制品中磺胺和喹诺酮类药物残留的方法。试样加入乙腈沉淀蛋白,用0.22μm滤膜过滤,经EndeavorsilTMC18柱分离,选用乙腈–0.1%甲酸为流动相。在0.05~100.00μg/L范围内,17种兽药的质量浓度均与色谱峰面积均呈良好的线性,相关系数(r2)为0.990 6~0.999 8,方法检出限为0.05~0.10μg/kg,加标回收率为75.88%~116.00%,测定结果的相对标准偏差为1.5%~13%(n=5)。该方法快速、灵敏,可以满足对乳制品中多种兽药残留的快速检测要求。

Simultaneous Analysis of Sulfonamides and Quinolones in Milk and Milk Powder by UFLC-MS/MS

Sulfonamides and quinolones in milk products were determined by ultra-performance liquid chromatography-tandem mass spectrometry. The proteins in milk products were precipitated by acetonitrile,then cleaned by 0.22μm millipore filter. The filtrate was separated on a EndeavorsilTMC18 column by gradient elution with acetonitrile-0.1% formic acid as mobile phase. In the range of 0.05-100.00μg/L, mass concentration of 17 veterinary drugs was linear with peak area with correlation coefficient (r2) of 0.9906-0.9998. The detection limit was 0.05-0.10μg/kg. The recoveries ranged from 75.88% to 116.00%,and the relative standard deviations were in the range of 1.5%-13%(n=5). The method is rapid and accurate,it can meet the requirements of monitoring of antibiotics in milk products.