【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。更多还原

【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.更多还原