超高效液相色谱-串联质谱法测定奶酪中喹乙醇及其代谢物

Determination of olaquindox and its metabolite in cheese by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  喹乙醇  3-甲基-喹噁啉-2-羧酸  奶酪  超高效液相色谱-串联质谱法

英文关键词:olaquindox  methyl-3-quinoxaline-2-carboxylic acid  cheese  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-串联质谱法测定奶酪中喹乙醇及其代谢物3-甲基-喹噁啉-2-羧酸(3-methyl-quinoxaline-2-carboxylic acid, MQCA)的含量。方法 样品经盐酸水解, 乙酸乙酯-乙腈提取、富集, 以乙腈-0.05%氨水为流动相, 经Inertsil ODS-3色谱柱分离, 采用多反应监测正离子模式进行定性及定量分析。结果 喹乙醇和3-甲基-喹噁啉-2-羧酸的检出限分别为0.05 μg/kg和0.02 μg/kg, 3个水平加标回收率为70.0%~109.0%, 相对标准偏差分别为10.55%和4.73%。结论 该方法具有灵敏度高、重复性好、准确度高、样品前处理操作简便和检测速度快的优点, 适用于奶酪中喹乙醇及其代谢物残留的检测。

英文摘要:

      Objective To establish a method for determination of olaquindox and its metabolite 3-methyl-quinoxaline-2-carboxylic acid (MQCA) in cheese by ultra performance liquid chromatography-tandem mass spectrometry. Methods The cheese sample was hydrolyzed by hydrochloric acid and extracted with ethyl acetate-acetonitrile for the enrichment of target compounds. Target compounds were separated with Inertsil ODS-3 column using acetonitrile-water (0.05% ammonia) as mobile phase, and the qualitative and quantitative analysis was carried out by mass spectrometry in the positive electrospray ionization under multiple reaction monitoring mode (MRM). Results The detection limits of olaquindox and MQCA were 0.05 μg/kg and 0.02 μg/kg, the recoveries were 70.0%-109.0% at 3spiked levels, and the relative standard deviations were 10.55% and 4.73%, respectively. Conclusion The method has the advantages of higher sensitivity, good repeatability, higher accuracy, convenient operation and shorter analysis time, and thus is suitable for the detection of olaquindox and its metabolite in cheese.