食品科学

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高效液相色谱光化学在线衍生荧光法检测鸡肉中16 种磺胺类药物残留

许 旭1,2,耿丹丹1,2,迟晓峰1,董 琦1,胡风祖1,*,肖远灿1,*   

  1. 1.中国科学院西北高原生物研究所,青海 西宁 810008;2.中国科学院大学生命科学院,北京 100049
  • 出版日期:2015-11-25 发布日期:2015-12-03
  • 通讯作者: 胡风祖,肖远灿
  • 基金资助:

    中国科学院仪器功能开发技术创新项目(Ig201308);中国科学院知识创新工程重要方向项目(KSCX2-EW-J-26);
    青海省科技平台建设项目(2012-T-Y19)

Determination of 16 Sulfonamide Residues in Chicken by High Performance Liquid Chromatography with Online Photochemical Derivatization and Fluorescence Detection

XU Xu1,2, GENG Dandan1,2, CHI Xiaofeng1, DONG Qi1, HU Fengzu1,*, XIAO Yuancan1,*   

  1. 1. Northwest Institute of Plateau Biology, Chinese Academy of Sciences, Xining 810008, China;
    2. College of Life Science, University of Chinese Academy of Science, Beijing 100049, China
  • Online:2015-11-25 Published:2015-12-03
  • Contact: HU Fengzu, XIAO Yuancan

摘要:

采用高效液相色谱-光化学柱后在线衍生-荧光检测法检测鸡肉中16 种磺胺类药物残留量。鸡肉样品经过乙腈提取并脱脂净化,色谱柱分离,光化学在线衍生并直接用荧光检测器检测。流动相为0.3%的冰乙酸和甲醇溶液梯度洗脱,流速0.7 mL/min、柱温36 ℃,激发波长320 nm、发射波长450 nm,16 种磺胺类药物得到良好分离。16 种磺胺药物在0.13~67.89 μg/mL质量度范围内,线性良好(R≥0.994 0),回收率在61.2%~106.6%之间,相对标准偏差为0.3%~13.9%,检出限为1.0~67.4 μg/kg。该方法灵敏、准确、快速,可满足鸡肉中磺胺类残留的检测。

关键词: 鸡肉, 磺胺类药物, 光化学在线衍生, 高效液相色谱-荧光检测

Abstract:

A high performance liquid chromatography (HPLC) with online postcolumn photochemical derivatization and
fluorescence detection (FLD) method was established for the determination of 16 sulfonamide residues in chicken. Chicken
samples were extracted with acetonitrile and the extract was defatted, separated by column chromatography, treated by online
photochemical derivatization and detected using a fluorescence detector. The mobile phase was a mixture of 0.3% glacial
acetic acid and methanol solution at a flow rate of 0.7 mL/min. The column temperature was set as 36 ℃, and the excitation
and emission wavelengths were set as 320 and 450 nm, respectively. The 16 sulfonamide residues were successfully
separated and determined under chosen experimental conditions. The calibration curves showed good linearity in the range
of 0.13–67.89 μg/mL (R ≥ 0.994 0). The recovery rates of the 16 sulfonamide residues were in the range of 64.3%–106.6%
with relative standard deviation (RSD) of 0.3%–13.9%.The limits of detection (LOD) for the sulfonamides were 1–
67.4 μg/kg. The established method is sensitive, accurate, rapid, and suitable for the determination of sulfonamide residues
in chicken.

Key words: chicken, sulfonamides, online photochemical derivatization, HPLC-FLD

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