超高效液相色谱串联质谱法测定鸡蛋中喹乙醇及卡巴氧代谢物

Determination of metabolites of olaquindox and carbadox in egg by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱串联质谱法  3-甲基-喹恶啉-2-羧酸  喹恶啉-2-羧酸  鸡蛋

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  methyl-3-quinoxaline-2-c arboxylic acid  quinoxaline-2-carboxylic acid  egg

中文摘要:

      目的 建立超高效液相色谱串联质谱法检测鸡蛋中喹乙醇代谢物3-甲基-喹恶啉-2-羧酸以及卡巴氧代谢物喹恶啉-2-羧酸的分析方法。方法 样品经酶解后, 用乙酸乙酯提取, PAX固相萃取柱净化, 用色谱柱WATERS ACQUITY UPLC HSS T3(2.1 mm×100 mm, 1.8 μm)分离, 同位素内标法定量。结果 3-甲基-喹恶啉-2-羧酸及喹恶啉-2-羧酸的最低检出限均为0.2 μg/kg, 定量限均为0.6 μg/kg, 平均回收率为80.9%~106.4%, 相对标准偏差为2.6%~7.2%。结论 该方法净化效果好, 灵敏度高, 准确性好, 适用于鸡蛋中喹乙醇以及卡巴氧代谢物的同时检测。

英文摘要:

      Objective To establish a method for the determination of methyl-3-quinoxaline-2-carboxylic acid and quinoxaline-2-carboxylic acid in egg by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods After enzymatic hydrolysis, the samples were extracted with ethyl acetate, followed by clean-up with PAX column, then separated by WATERS ACQUITY UPLC HSS T3(2.1 mm×100 mm, 1.8 μm). Internal standard method was used to quantify. Results The limits of detection and the limits of quantify were 0.2 μg/kg and 0.6 μg/kg for methyl-3-quinoxaline-2-carboxylic acid and quinoxaline-2-carboxylic acid, respectively. The recoveries were 80.9%-106.4% and the relative standard deviations (RSDs) were 2.6%-7.2%. Conclusion This method has good purification, high sensitivity, good accuracy, and is suitable for determination of methyl-3-quinoxaline-2-carboxylic acid and quinoxaline-2-carboxylic acid in egg.