星点设计-响应面法优化肉桂油β-环糊精包合物制备工艺

Optimization of Preparation Technology of Inclusion Complex of Oil from Cinnamon and β-Cyclodextrin by Central Composite Design-response Surface Methodology

目的:优化肉桂油β-环糊精包合物(β-CD)的制备工艺。方法:采用研磨法制备肉桂油β-CD包合物。以包合物中桂皮醛含量为评价指标,采用星点设计-响应面法考察包合比例、包合温度和包合时间对肉桂油β-环糊精包合物制备工艺的影响,对试验数据进行多元线性回归和二项式方程拟合,通过效应面法优选包合工艺并进行预测分析。以高效液相色谱法(HPLC)和热重差热分析法(TG-DTA)对该包合物进行质量评价。结果:肉桂油β-CD包合物制备的最佳包合工艺为β-CD与肉桂油的包合比例(g/g)10∶1,包合温度50℃,包合时间58 min。包合物中桂皮醛含量预测值为10.21%。实际值测得包合物中桂皮醛平均含量为10.10%,与预测值的偏差依次为:0.68%,1.56%和0.98%。结论:HPLC和TG-DTA分析表明肉桂油包合物已制备成功,采用星点设计-响应面法优化肉桂油β-环糊精包合物制备工艺,方法简便,可预测性良好,为肉桂油的应用提供科学依据。

Objective： To optimize the preparation process of inclusion complex of oil from cinnamon and β-Cyclodextrin（ β-CD）.Method： Cinnamon oil β-CD inclusion complex was prepared by trituration method. Taking the content of cinnamaldehyde as index,central composite design-response surface methodology was adopted to optimize inclusion process with mass ratio of cinnamon oil andβ-CD,inclusion temperature and reaction time as factors,test data were fitted by multi-linear equation and second-order polynomial equation,optimal inclusion technology was predicted by response surface method. The quality of inclusion complex was evaluated by HPLC and TG-DTA. Results： The best process was as follows,mass ratio of cinnamon oil and β-CD was 10∶ 1,inclusion temperature was 50℃,inclusion time was 58 min. The predicted value of cinnamaldehyde content in inclusion compound was 10. 21%. The average content of cinnamaldehyde in the inclusion compound was 10. 10%,and the deviations from the predicted values were 0. 68%,1. 56% and 0. 98%,respectively. Conclusion： The characterization results of HPLC and TG-DTA proved the generation of inclusion complex. Optimization of preparation technology of inclusion complex of oil from cinnamon and β-CD by central composite design-response surface methodology,the methods was simple,good predictability and provide scientific basis for the application of cinnamon oil.