响应曲面法优化仲丁胺气相色谱检测的衍生条件.pdfVIP

※分析检测 食品科学 2012, Vol. 33, No. 08 211 纪淑娟，于兰洁，刘 玲，白 冰，周 丹 (沈阳农业大学食品学院，辽宁 沈阳 110866) 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 。 仲丁胺；残留；衍生；响应曲面法；气相色谱 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 (College of Food, Shenyang Agricultural University, Shenyang 110866, China) 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 0.05 μL/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 中图分类号：TS207.3 文献标识码：A 文章编号：1002-6630(2012)08-0211-05 仲丁胺(sec-butylamine ，2-AB) ，分子式为CH3CH 腐保鲜剂，目前，主要应用于柑橘、柠檬、苹果、 ( N H 2 ) C 2 H 5 ，是具有对映异构现象的简单二级胺，有 蒜薹、青椒等果品蔬菜的贮运保鲜。GB 2760 — 2011 刺激性