色谱

色谱 ›› 2012, Vol. 30 ›› Issue (07): 660-664.DOI: 10.3724/SP.J.1123.2012.02018

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法测定动物源食品中3-甲基喹喔啉-2-羧酸和喹喔啉-2-羧酸残留

郑玲, 吴玉杰, 李湧, 李丽华   

  1. 广西出入境检验检疫局, 广西 南宁 530021
  • 收稿日期:2012-02-17 修回日期:2012-03-29 出版日期:2012-07-28 发布日期:2012-07-19
  • 通讯作者: 吴玉杰
  • 基金资助:

    国家质量监督检验检疫总局科研项目(2009IK146).

Determination of the residues of 3-methyl-quinoxaline-2-carboxylic acid and quinoxaline-2-carboxylic acid in animal origin foods by high performance liquid chromatography-tandem mass spectrometry

ZHENG Ling, WU Yujie*, LI Yong, LI Lihua   

  1. Guangxi Entry-Exit Inspection and Quarantine Bureau, Nanning 530021, China
  • Received:2012-02-17 Revised:2012-03-29 Online:2012-07-28 Published:2012-07-19
  • Contact: 吴玉杰,博士,高级工程师,研究方向为食品安全.

PDF

418

被引次数

18

摘要： 建立了动物源食品中喹喔啉类药物代谢残留标识物3-甲基喹喔啉-2-羧酸和喹喔啉-2-羧酸的高效液相色谱-串联质谱检测方法。样品在酸性环境水解,经乙酸乙酯、磷酸盐缓冲液依次提取,Oasis MAX固相萃取小柱净化,用Waters Xterra MS C18柱(150 mm×2.1 mm, 5 μm)分离,以甲醇-0.2%甲酸为流动相梯度洗脱,采用多反应监测(MRM)正离子模式检测,内标法定量。各物质在1.0～20.0 μg/L范围内线性关系良好,相关系数均不低于0.9996; 3-甲基喹喔啉-2-羧酸和喹喔啉-2-羧酸在0.1、0.2、1.0 μg/kg加标水平的回收率为62.4%～118%,相对标准偏差为1.48%～28.1%;定量限(以信噪比≥10计)为0.1 μg/kg。该方法简单、灵敏、稳定,可满足猪肉、猪肝、鸡肉、鸡肝、鱼、虾等动物源食品中3-甲基喹喔啉-2-羧酸和喹喔啉-2-羧酸残留的检测与确证需要。

关键词: 3-甲基喹喔啉-2-羧酸, 动物源食品, 高效液相色谱-串联质谱, 喹喔啉-2-羧酸

Abstract: A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the simultaneous quantitative determination of 3-methyl-quinoxaline-2-carboxylic acid (MQCA) and quinoxaline-2-carboxylic acid (QCA) as the marker residues for carbadox (CBX) and olaquindox (OLA), respectively, in the muscles and livers of porcine and chicken and in the muscles of fish and shrimp. The MQCA and QCA were deproteinated with 5% metaphosphoric acid in 10% methanol followed by liquid-liquid extraction. Further clean-up was performed by solid phase extraction (SPE) through mixed mode anion-exchange columns (Oasis MAX SPE). The separation of the compounds was carried on a Waters Xterra MS C18 column (150 mm×2.1 mm, 5 μm) by a gradient elution using methanol and 0.2% formic acid as mobile phases. The analytes were detected by tandem mass spectrometry in multiple reaction monitoring (MRM) mode with positive electrospray ionization. The MQCA and QCA were quantified by internal standard method. The linear ranges were 1.0~20.0 μg/L and the correlation coefficients were not less than 0.9996. The average recoveries and relative standard deviations ranged from 62.4%~118% and 1.48%~28.1% respectively at the spiked levels of 0.1, 0.2 and 1.0 μg/kg for the both markers. The limit of quantitation (LOQ) was 0.1 μg/kg. The method is sensitive, accurate and suitable for the determination and confirmation of MQCA and QCA in animal origin foods.

Key words: 3-methyl-quinoxaline-2-carboxylic acid (MQCA) , animal origin foods, quinoxaline-2-carboxylic acid(QCA) , high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS)