色谱

色谱

• 技术与应用 • 上一篇    下一篇

高效液相色谱荧光检测法测定蔬菜中残留的甲氨基阿维菌素苯甲酸盐

张艳1,3,吴银良2,胡继业4,王宏卫1,潘灿平3,刘丰茂3

  

  1. 1.Beijing Huadu Broiler Corporation, Beijing 102211, China; 2.Quality Control and Inspection Center for
    Domestic Animal Products of MOA, Beijing 100026, China; 3.College of Science, China Agricultural
    University, Beijing 100094, China; 4.Research Center for Eco-environmental Sciences,
    the Chinese Academy of Sciences, Beijing 100085, China
  • 收稿日期:2007-06-05 修回日期:2007-10-23 出版日期:2008-01-30 发布日期:1984-09-25
  • 通讯作者: 吴银良

Determination of emamectin benzoate residue in vegetables by high performance liquid chromatography
with fluorescence detection

ZHANG Yan1,3, WU Yinliang2, HU Jiye4, WANG Hongwei1, PAN Canping3, LIU Fengmao3   

  1. 1.Beijing Huadu Broiler Corporation, Beijing 102211, China; 2.Quality Control and Inspection Center for
    Domestic Animal Products of MOA, Beijing 100026, China; 3.College of Science, China Agricultural
    University, Beijing 100094, China; 4.Research Center for Eco-environmental Sciences,
    the Chinese Academy of Sciences, Beijing 100085, China
  • Received:2007-06-05 Revised:2007-10-23 Online:2008-01-30 Published:1984-09-25

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摘要：

建立了甘蓝和蘑菇中甲氨基阿维菌素苯甲酸盐的固相萃取-高效液相色谱荧光分析方法。蔬菜样品用乙酸乙酯提取,提取液旋转浓缩近干后用少量乙酸乙酯溶解,再经PRS固相萃取(SPE)柱净化,洗脱液经氮气吹干后用氮甲基咪唑和三氟乙酸酐衍生,衍生物用高效液相色谱分析,采用外标法定量。在添加浓度1.0～20.0 μg/kg范围内,平均添加回收率为78.6%～84.9%,日内相对标准偏差(RSD)为2.7%～6.0%,日间RSD为3.1%～8.9%,检出限为0.10 μg/kg。甲氨基阿维菌素苯甲酸盐衍生物在0.002～0.10 mg/L范围内呈良好的线性关系,相关系数为0.9999。

关键词: 残留, 高效液相色谱法, 固相萃取, 甲氨基阿维菌素苯甲酸盐, 蔬菜

Abstract:

A method was developed for the determination of emamectin benzoate residue in cabbage and mushroom using solid-phase extraction (SPE) and high performance liquid chromatography (HPLC) with fluorescence detection. The sample was extracted with ethyl acetate. Further cleanup was performed on a propylsulfonic acid solid phase extraction cartridge, followed by the derivatization with trifluoroacetic anhydride in the presence of N-methylimidazole. The amount of derivatized emamectin benzoate was determined by fluorescence detector after separation by HPLC. The detection limit was 0.10 μg/kg for cabbage and mushroom samples. The recoveries of emamectin benzoate in cabbage and mushroom samples were 78.6%-84.9%. The inter-day relative standard deviation (RSD) and intra-day RSD were 2.7%-6.0% and 3.1%-8.9%, respectively, at the fortified levels of 1.0-20.0 μg/kg. The calibration curve of emamectin benzoate in vegetables at the concentration range of 0.002 mg/L to 0.10 mg/L was linear (r=0.9999).

Key words: emamectin benzoate, residue, solid-phase extraction (SPE), vegetable
, high performance liquid chromatography (HPLC)