食品与发酵工业 >

2021 , Vol. 47 >Issue 19: 252 - 257

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.026319

分析与检测

QuEChERS结合HPLC-MS/MS同时测定鱼肉中多种兽药残留

  • 刘进玺 ,
  • 王铁良 ,
  • 胡京枝 ,
  • 杨亚琴 ,
  • 冯慧慧 ,
  • 钟红舰
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  • (河南省农业科学院 农业质量标准与检测技术研究所,农业部农产品质量监督检验测试中心,农业部农产品质量安全风险评估重点实验室,河南 郑州,450002)
硕士,副研究员(钟红舰研究员为通讯作者,E-mail: 80456811@163.com)

收稿日期: 2020-12-03

  修回日期: 2021-01-15

  网络出版日期: 2021-11-04

基金资助

河南省农业科学院自主创新基金项目(2018ZC 66);河南省市场监督管理局关于印发河南省2019年食品安全风险监测计划的通知(豫市监【2019】112号);农业农村部农产品质量安全监管(风险评估)专项农质发【2019】10号

收起

Determination of veterinary drug residues in fish by QuEChERS method with HPLC-MS/MS

  • LIU Jinxi ,
  • WANG Tieliang ,
  • HU Jingzhi ,
  • YANG Yaqin ,
  • FENG Huihui ,
  • ZHONG Hongjian
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  • (Institute of Agricultural Quality Standards and Testing Technology,Henan Academy of Agricultural Science, Supervision and Test Center of Agricultural Product Quality,Ministry of Agriculture,Laboratory of Quality and Safety Risk Assessment for Agricultural Product,Zhengzhou 450002,China)

Received date: 2020-12-03

  Revised date: 2021-01-15

  Online published: 2021-11-04

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摘要

利用液相色谱-质谱法建立了鱼肉中磺胺类、喹诺酮类、酰胺醇类、硝基咪唑类、地西泮和孔雀石绿药物多残留的检测技术。样品用甲酸乙腈和Na2EDTA-Mcllvaine缓冲溶液提取,经C18和无水硫酸镁吸附净化,以C18色谱柱(2.0 mm×100 mm×3 μm)分离,在正负多反应模式下监测采集,外标法定量。25种兽药在0.1～200 μg/L相关系数良好,相关系数(r)>0.99;在2、4、10 μg/kg 3个浓度水平下加标回收的平均回收率为71.8%～107%,相对标准偏差为4.2%～9.2%。对工作中检出的鱼类阳性样品,使用该文所建立的方法和标准方法采用F检验进行单因素方差分析,结果表明,2种方法的测定结果无显著性差异(P<0.05)。

关键词： 检测; 兽药残留; 鱼肉; 液相色谱-串联质谱

本文引用格式

刘进玺 , 王铁良 , 胡京枝 , 杨亚琴 , 冯慧慧 , 钟红舰 . QuEChERS结合HPLC-MS/MS同时测定鱼肉中多种兽药残留[J]. 食品与发酵工业, 2021 , 47(19) : 252 -257 . DOI: 10.13995/j.cnki.11-1802/ts.026319

Abstract

A method was established for the determination of veterinary drugs (sulfonamides, quinolones, amide alcohols, imidazole nitrate, diazepam and malachite green) in fish by liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The samples were extracted with formic acid acetonitrile and Na2EDTA-Mcllvaine buffer solution and then purified by C18 and anhydrous MgSO4. The residues were separated on a C18 column (2.0 mm×100 mm×3 μm), the MS data was acquired in positive and negative multiple reaction monitoring (MRM) modes, and quantitated by the external standard method. With this approach, the linear relationship of the 25 veterinary drugs was good, and the linear correlation coefficients were greater than 0.99 in the range of 0.1-200 μg/L. The average recoveries at three spiked levels (2, 4 and 10μg/kg) were 71.8%-107% with relative standard deviations of 4.2%-9.2%. In actual work, for those positive fish samples, at the significance level of 0.05, there was no significant difference between the standard method and the method developed in this article.

Key words： detection; veterinary drug residue; fish; liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)

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