蛋 奶及其制品中多种兽药残留的同步快速筛查

Simultaneous Rapid Screening of Multiple Veterinary Drug Residues in Eggs Milk and its Products

通过优化改进前处理过程,建立同时快速筛查蛋、奶及其制品中抗菌类和抗病毒类药物残留的超高效液相色谱-质谱联用方法(UPLC-MS/MS)。均质后的样品,经酸化乙腈提取,无水硫酸钠除水,用UPLC-MS/MS进行检测,金刚烷胺和金刚乙胺采用内标法定量,磺胺类和喹诺酮类采用外标法定量。结果表明,在不同基质下,6种兽药残留在1~50 ng/mL质量浓度范围内均呈现良好的线性关系,且相关系数R2均在0.995以上。分别对蛋和奶进行3个质量浓度水平的加标试验,得到其回收率为75.9%~117.5%,相对标准偏差RSD均小于15%。该方法操作简单、分析快速、稳定性好,适合大批量蛋、奶及其制品中磺胺类、喹诺酮类和金刚烷胺、金刚乙胺药物残留的同步快速筛查。

By optimizing and improving the pre-experimental treatment process,an ultra-high performance liquid chromatogram-mass spectrometry(UPLC-MS/MS)method was established for simultaneous rapid screening of multiple antibacterial and antiviral drug residues in eggs,milk and its products.The homogenized samples were extracted by acidified acetonitrile,dehydrated by anhydrous sodium sulfate,and detected by UPLC-MS/MS.Amantadine and rimantadine were quantified by internal standard method,and sulfonamides and quinolones were quantified by external standard method.The results showed that under different substrates,the six veterinary drug residues showed a good linear relationship in the concentration range of 1~50 ng/mL,and the R2 all above 0.995.The negative samples of egg and milk were spiked at three concentration levels respectively,and the recoveries were found to be in the range of 75.9%~117.5%,with RSD less than 15%.This method was simple,rapid and stable,and suitable for simultaneous rapid screening of sulfonamides,quinolones,amantadine and rimantadine residues in large quantities of eggs,milk and its products.