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 chromatographytandem mass spectrometry

作　　者：张嘉慧[1] 沈祥广[1] 刘戎[1] 刘晓晖 林杰 刘文字[1] ZHANG Jia-Hui;SHEN Xiang-Guang;LIU Rong;LIU Xiao-Hui;LIN Jie;LIU Wen-Zi(Animal and Poultry Products Quality Control,Inspection and Testing Center(Guangzhou),Ministry of Agriculture and Rural Affairs,College of Veterinary Medicine,South China Agriculture University,Guangzhou 510642,China)

机构地区：[1]华南农业大学兽医学院,农业农村部畜禽产品质量监督检验测试中心(广州),广州510642

出　　处：《食品安全质量检测学报》2021年第9期3764-3770,共7页Journal of Food Safety and Quality

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0.5~100μg/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0.5μg/kg;喹乙醇残留标示物3-甲基喹噁啉-2-羧酸在0.5、5.0、20μg/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。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 0.5-100μg/L,and the correlation coefficient r was greater than 0.99.The detection limit and quantitation limit of the method were both 0.5μg/kg.The recoveries of 3-methylquinoxaline-2-carboxylic acid at the 0.5,5.0,and 20μg/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.

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 

分 类 号：O657.63[理学—分析化学] TS251.7[理学—化学]