畜牧与饲料科学 ›› 2020, Vol. 41 ›› Issue (3): 76-79.doi: 10.12160/j.issn.1672-5190.2020.03.015

• 兽医药物科学 • 上一篇    下一篇

液质联用法检测禽蛋中氟苯尼考和氟苯尼考胺残留

李雅宁, 苏亚, 郭林云   

  1. 内蒙古自治区兽药监察所,内蒙古 呼和浩特 010010
  • 收稿日期:2020-04-08 出版日期:2020-05-30 发布日期:2020-06-17
  • 通讯作者: 苏亚(1979—),女,高级兽医师,主要研究方向为兽药残留检验。
  • 作者简介:李雅宁(1990—),女,硕士,主要研究方向为兽药残留检验。
  • 基金资助:
    福建省科技计划引导性项目(2019Y6005);福建省科学技术厅创新资金项目(2018C0041);福建省软科学研究项目(2018ER019)。

Determination of Florfenicol and Florfenicol Amine Residues in Poultry Eggs by UPLC-MS/MS

LI Ya-ning, SU Ya, GUO Lin-yun   

  1. Inner Mongolia Institute of Veterinary Drug Control,Hohhot 010010,China
  • Received:2020-04-08 Online:2020-05-30 Published:2020-06-17

摘要: 建立了超高效液相色谱串联质谱法检测禽蛋中氟苯尼考和氟苯尼考胺残留物的方法。采用电喷雾离子源(ESI)、多反应监测(MRM)、正负离子模式同时扫描检测,内标法定量。禽蛋试样采用碱化乙酸乙酯和乙腈提取,正己烷萃取,LC/MS-MS分析。结果表明,该方法的检测限(LODs)为0.1 μg/kg,定量限(LOQs)为0.2 μg/kg。在0.2~200 μg/L范围内均呈良好线性关系,并且3个添加浓度的平均回收率范围为70%~110%,相对标准偏差(RSD)小于10%。该方法简便高效、准确可靠,可作为禽蛋中氟苯尼考和氟苯尼考胺残留的检测方法。

关键词: 禽蛋, 氟苯尼考, 氟苯尼考胺, 超高效液相色谱—串联质谱;

Abstract: In this study, an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC/MS-MS) method for determination of florfenicol and florfenicol amine residues in poultry eggs was established. The electrospray ion source (ESI), multiple reaction monitoring (MRM), and positive and negative ion mode were simultaneously used for scanning and detection, and the internal standard method was used for quantitative analysis. Poultry egg samples were extracted with ethyl acetate and acetonitrile after alkalization, then extracted with n-Hexane, and finally analyzed by UPLC/MS-MS. The results showed that the detection limit (LODs) of the established method was 0.1 μg/kg, and the quantification limit (LOQs) was 0.2 μg/kg. There was a good linear relationship in the range of 0.2-200 μg/L, the average recovery rates of the three added concentrations were 70%-110%, and the relative standard deviation (RSD) was less than 10%. In conclusion, the UPLC-MS/MS method established in this study is simple, efficient, accurate and reliable, and can be used for determination of florfenicol and florfenicol amine residues in poultry eggs.

Key words: poultry eggs, florfenicol, florfenicol amine, UPLC-MS/MS

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