液相色谱-串联质谱法测定猪肝中喹乙醇残留标示物3-甲基喹噁啉-2-羧酸

Determination of 3-methyl quinoxaline-2-carboxylic acid of olaquindox marker residue in porcine liver by liquid chromatography- tandem mass spectrometry

中文关键词:  喹乙醇  液相色谱-串联质谱法  3-甲基喹噁啉-2-羧酸  猪肝样品  残留

英文关键词:olaquindox  liquid chromatography-tandem mass spectrometry  3-methylquinoxaline-2-carboxylic acid  porcine liver  residue

中文摘要:

      目的 建立液相色谱-串联质谱法测定猪肝中喹乙醇残留标示物3-甲基喹噁啉-2-羧酸(3-methylquinoxaline-2-carboxylic acid, MQCA)含量的分析方法。方法 猪肝匀浆中的喹乙醇标示物3-甲基喹噁啉-2-羧酸经乙腈提取, MAX固相萃取柱净化, 2%的甲酸乙酸乙酯溶液洗脱收集, 浓缩定容。分析样品采用C18色谱柱分离, 以乙腈、0.1%甲酸溶液为流动相, 多反应离子监测(multiple reaction monitoring, MRM)模式测定, 内标法定量。结果 喹乙醇残留标示物3-甲基喹噁啉-2-羧酸在0.5~100 μg/L浓度范围内线性良好, 相关系数r大于0.99; 该方法的检出限和定量限均为0.5 μg/kg; 喹乙醇残留标示物3-甲基喹噁啉-2-羧酸在0.5、5.0、20 μg/kg添加水平的回收率为97.7%~101.4%, 相对标准偏差小于3.54%。结论 该方法简单快速、准确、灵敏, 适用于猪肝中喹乙醇残留标示物3-甲基喹噁啉-2-羧酸的快速检测。

英文摘要:

      Objective To establish an analytical method for the determination of 3-methylquinoxaline- 2-carboxylic acid of olaquindox marker residue in porcine liver by liquid chromatography-tandem mass spectrometry. Methods Olaquindox 3-methylquinoxaline-2-carboxylic acid in porcine liver homogenate was extracted with acetonitrile, purified by a MAX solid-phase extraction column, eluted with 2% ethyl formate solution, collected, and concentrated to a constant volume. The analytical samples were separated on a C18 column using acetonitrile and 0.1% formic acid solution as the mobile phase, determined by multiple reaction monitoring (MRM) mode and quantified by internal standard method. Results The linearity of olaquindox residual marker 3-methylq uinoxaline-2-carboxylic acid was good in the concentration range of 0.5?100 μg/L, and the correlation coefficient r was greater than 0.99. The detection limit and quantitation limit of the method were both 0.5 μg/kg. The recoveries of 3-methylquinoxaline-2-carboxylic acid at the 0.5, 5.0, and 20 μg/kg addition levels were 97.7%?101.4%, and the relative standard deviations were less than 3.54%. Conclusion This method is simple, rapid, accurate and sensitive, and is suitable for the rapid detection of 3-methylquinoxaline-2-carboxylic acid, a marker of olaquindox residues in porcine liver.