超高效液相色谱-串联质谱法测定畜肉中喹乙醇和代谢物残留及其冷冻储藏稳定性研究

Determination of olaquindox and its metabolite residues in meat by ultra performance liquid chromatography-tandem mass spectrometry and the study on their frozen storage stability

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

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

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定畜肉中喹乙醇(olaquindox, Ola)及其代谢物3-甲基-喹噁啉-2-羧酸(3-methyl-quinoxaline-2-carboxylic acid, MQCA)残留量的检测方法, 并研究在冷冻储藏条件下畜肉中Ola及MQCA的稳定性。方法 采用碱性水解提取畜肉中Ola及MQCA, 经混合型阴离子交换固相萃取柱净化, 以乙腈和0.2%甲酸溶液为流动相, 经C18色谱柱洗脱分离, 电喷雾正离子模式电离, 多反应监测(multiple reaction monitoring, MRM)模式检测, 外标法定量; 通过降解率, 分析畜肉中Ola和MQCA在冷冻储藏条件下的稳定性。结果 Ola及MQCA在0.5~100.0 μg/kg范围内, 质谱响应强度与其质量浓度呈良好的线性关系, 相关系数(r)≥0.9996; 检出限均为0.1 μg/kg, 定量限均为0.5 μg/kg; 加标回收率为92.7%~98.6%, 相对标准偏差为1.2%~3.7%; Ola及MQCA在-20 ℃储藏180 d是稳定的。结论 该法样品前处理操作简单、准确度高、精度好, 可为畜肉中Ola及MQCA残留量检测提供方法。

英文摘要:

      Objective To establish a method for the determination of olaquindox (Ola) and its metabolite 3-methyl-quinoxaline-2-carboxylic acid (MQCA) by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), and study the stability of Ola and MQCA in livestock meat under frozen storage conditions. Methods Ola and MQCA from animal meat were extracted by using alkaline hydrolysis, purified by mixed anion exchange solid phase extraction column, using acetonitrile and 0.2% formic acid solution as mobile phase, eluted and separated by C18 chromatographic column, ionizated by electrospray positive ion mode, detected by multiple reaction monitoring (MRM) mode, and quantified by external standard method. Storage stability of Ola and its metabolite MQCA in livestock meat under freezing conditions was also investigated. Results The results showed that the mass concentration of Ola and MQCA showed a good linear relationship with the mass spectrometry response value in the range from 0.5 μg/kg to 100.0 μg/kg, and the correlation coefficient (r) were not less than 0.9996. The limits of detection were 0.1 μg/kg, the limits of quantitation were 0.5 μg/kg, the recoveries rates were in the range from 92.7% to 98.6%, and the relative standard deviations were in the range from 1.2% to 3.7%. Ola and MQCA were stable when stored at ?20 ℃ for 180 days. Conclusion This method has the advantages of simple pretreatment, high accuracy and good precision, and can provide a method for the detection of Ola and MQCA residues in livestock meat.