食品科学 ›› 2012, Vol. 33 ›› Issue (8): 211-215.doi: 10.7506/spkx1002-6630-201208046

• 分析检测 • 上一篇    下一篇

响应曲面法优化仲丁胺气相色谱检测的衍生条件

纪淑娟,于兰洁,刘 玲,白 冰,周 丹   

  1. 沈阳农业大学食品学院
  • 出版日期:2012-04-25 发布日期:2012-03-31
  • 基金资助:
    农业部行业标准制定项目(2130109)

Optimization of Derivatization Conditions for Gas Chromatographic Determination of Sec-Butylamine by Response Surface Methodology

JI Shu-juan,YU Lan-jie,LIU Ling,BAI Bing,ZHOU Dan   

  1. (College of Food, Shenyang Agricultural University, Shenyang 110866, China)
  • Online:2012-04-25 Published:2012-03-31

摘要: 利用响应面法优化仲丁胺气相色谱检测的衍生条件。根据Box-Behnken中心组合试验设计原理,针对试验中衍生化反应这一重要环节,在单因素试验基础上,以仲丁胺回收率为响应值,应用响应曲面法研究衍生反应时间、温度、衍生剂用量各因素间的交互作用及其对仲丁胺测定回收率的影响。以五氟苯甲醛溶液作为衍生剂,经气相色谱电子捕获检测器分析测定。确定最佳衍生条件为:衍生反应时间31.72min、衍生反应温度22.42℃、衍生剂用量1.25mL。

关键词: 仲丁胺, 残留, 衍生, 响应曲面法, 气相色谱

Abstract: Derivatization reaction is very important for the determination of sec-butylamine. For the purpose of establishing a gas chromatography-electron capture detection (GC-ECD) method for determining sec-butylamine, the optimal derivatization reaction conditions were studied by response surface methodology. Based on the results of one-factor-at-a-time experiments, a central composite design was used to investigate the pairwise interaction effects of reaction time, temperature and derivatization reagent (acetonitrile containing 0.05μL/mL pentafluorobenzaldehyde) amount on sec-butylamine recovery. The optimal derivative temperature, derivative duration and derivatization reagent amount were found to be 22.42 ℃, 31.72 min and 1.25 mL, respectively.

Key words: sec-butylamine, residue, derivatization, response surface methodology, gas chromatography

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