色谱

色谱 ›› 2019, Vol. 37 ›› Issue (10): 1059-1063.DOI: 10.3724/SP.J.1123.2019.04050

• 特别策划：固相萃取和QuEChERS应用专栏 • 上一篇    下一篇

高效液相色谱-串联质谱法检测猪肉中3-甲基喹喔啉-2-羧酸残留

魏敏芝1, 万建春2, 张富生1, 潘华1   

  1. 1.江西省农产品质量安全检测中心, 江西 南昌 330012;
    2.江西省食品检验检测研究院, 江西 南昌 330001
  • 收稿日期:2019-04-30 出版日期:2019-10-08 发布日期:2020-12-11
  • 通讯作者: 潘华,Tel:(0791)88509111,E-mail:18449807@qq.com.
  • 基金资助:
    江西省重点研发计划项目（20181BBF60027）.

Determination of 3-methyl-quinoxaline-2-carboxylic acid residue in pork by high performance liquid chromatography-tandem mass spectrometry

WEI Minzhi1, WAN Jianchun2, ZHANG Fusheng1, PAN Hua1   

  1. 1. Test Center for Agriculture Product Quality and Safety of Jiangxi Province, Nanchang 330012, China;
    2. Jiangxi Food Inspection and Testing Research Institute, Nanchang 330001, China
  • Received:2019-04-30 Online:2019-10-08 Published:2020-12-11
  • Supported by:
    Key Science and Technology Program Project of Jiangxi Province (No. 20181BBF60027).

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摘要： 建立了高效液相色谱-串联质谱同时定量和确证猪肉中3-甲基喹喔啉-2-羧酸（MQCA）残留量的检测方法。试样用0.3 mol/L盐酸溶液水解提取，加入乙腈和乙酸乙酯萃取，再用0.1 mol/L氢氧化钠溶液反萃取，阴离子交换固相萃取柱净化，经Agilent Eclipse Plus C18柱（50 mm×3.0 mm，1.8 μm）分离，采用液相色谱-串联质谱仪检测，基质匹配添加标准曲线定量。MQCA在1.0~50 μg/L范围内线性相关系数大于0.99，在0.5、1.0、5.0 μg/kg加标水平下其回收率为90.5%~119.6%，相对标准偏差为3.14%~4.22%。方法可用于猪肉中MQCA残留量的快速定量和确证检测。

关键词: 液相色谱-串联质谱, 触发式多反应监测, 确证, 3-甲基喹喔啉-2-羧酸, 猪肉

Abstract: A method was developed for the simultaneous quantitative and confirmatory determination of 3-methylquinoxaline-2-carboxylic acid (MQCA) residues in pork by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was hydrolyzed with 0.3 mol/L hydrochloric acid solution, and MQCA was extracted by water bath oscillation. MQCA was first extracted with acetonitrile and ethyl acetate and then re-extracted from the extraction solution with 0.1 mol/L sodium hydroxide solution. Then MQCA was purified by an anion exchange solid phase extraction column. The chromatographic separation was performed using an Agilent Eclipse Plus C18 column (50 mm×3.0 mm, 1.8 μm). The quantitative analysis was performed by the matrix matching addition method. The correlation coefficient of MQCA in the range of 1.0-50 μg/L was greater than 0.99. The recovery was 90.5%-119.6% at the spiked levels of 0.5, 1.0 and 5.0 μg/kg, and the relative standard deviation was 3.14%-4.22%. The method can be used for the rapid quantitative determination of 3-methylquinoxaline-2-carboxylic acid residues in pork.

Key words: high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), triggered multi-reaction monitoring, confirmation, 3-methyl-quinoxaline-2-carboxylic acid, pork

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