高效液相色谱-串联质谱法测定动物源食品中喹乙醇代谢物残留量

Determination of Olaquindox Metabolite Residues in Food Products of Animal Origin Using High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立动物源性食品中喹乙醇代谢残留标识物3-甲基喹喔啉-2-羧酸残留量的高效液相色谱串联质谱法。样品均质后,经Protease蛋白酶进行过夜酶解,加入盐酸酸化,离心,过滤后采用阴离子交换固相萃取柱Oasis MAX进行净化和富集。分析样品经Kinetex C18色谱柱分离,在高效液相色谱-串联质谱多反应监测模式下进行定性、定量分析,采用正离子扫描。6种测定样品中3-甲基喹喔啉-2-羧酸定量下限均为0.5μg/kg,鳗鱼、虾、鸡肉、猪肉、牛肉和猪肝在0.5、1.0、4.0μg/kg和10.0μg/kg四个添加水平的平均回收率在60.7%～107%之间,相对标准偏差(n=10)在4.59%～14.9%之间。本方法分析速度快、灵敏度高、重现性好,各项技术指标均满足国内外相关法规要求,适用于动物源性食品中喹乙醇代谢物3-甲基喹喔啉-2-羧酸残留的确证检测。

A high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） method was developed to determine the olaquindox metabolite marker 3-methyl-quinoxaline-2-carboxylic acid （MQCA） in food products of animal origin. Samples were homogenized, hydrolyzed with protease overnight, acidified by adding hydrochloric acid, centrifugated, filtrated, and then cleaned up and enriched using an Oasis MAX solid phase extraction cartridge. The chromatographic separation was performed on a Kinetex Clscolumn. The qualitative and quantitative analysis of MQCA was carried out using an HPLC-MS/MS system under positive ion multiple reaction monitoring （MRM） mode. The limits of quantification for MQCA in meats from 6 different animal species （eel, shrimp, chicken, pork, beef and porcine liver） were all 0.5μ g/kg. The average recoveries at four different spike levels： 0.5, 1.0, 4.0 pg/mg and 10.0 pg/kg were 60.7% -- 107% with relative standard deviation between 4.59% and 14.9% （n = 10）. This method was fast, sensitive and reproducible and all of its technical indexes could meet the requirements of domestic and international relevant standards. Therefore it is applicable for the determination and confirmation of MQCA residues in food products of animal origin.