星点设计-效应面法优化芹菜籽挥发油羟丙基-β-环糊精的包合工艺

Optimization of preparation process for celery seeds oil-hydroxypropyl-β-cyclodextrin inclusion complex by central composite design-response surface methodology

关键词:  芹菜籽挥发油  丁苯酞  星点设计-效应面法  包合工艺

Key words:  celery seed oil  butylphthalide  central composite design-response surface methodology  inclusion process

摘要:

[目的]优化芹菜籽挥发油-羟丙基-β-环糊精包合物的包合工艺，并对包合物进行表征及评价。[方法]采用冷冻干燥法包合芹菜籽挥发油，以丁苯酞的包合率、载药量为评价指标，计算综合评分OD值。对包合温度、包合时间和芹菜籽挥发油与羟丙基-β-环糊精的比例进行单因素考察，并设计三因素五水平的星点实验。对实验结果进行多元线性、二项式及三项式拟合，采用效应面法筛选出的最佳包合工艺进行验证实验。采用高效液相色谱法（HPLC）测定包合物中丁苯酞的含量，采用紫外扫描法（UV）、差示扫描量热法（DSC）对芹菜籽挥发油-羟丙基-β-环糊精包合物进行表征。[结果]芹菜籽挥发油包合物的最优制备工艺为：芹菜籽挥发油：羟丙基-β-环糊精比例2：25、包合温度为44.5℃、包合时间167 min。此包合工艺制备的挥发油包合物包合率为78.95%，包合物中丁苯酞质量分数为2.982 mg/g。表征结果显示芹菜籽挥发油被羟丙基-β-环糊精成功包合。[结论]星点设计-效应面法适用于芹菜籽挥发油-羟丙基-β-环糊精的包合工艺优化，此方法建立的数学模型具有良好的预测性。

Abstract:

[Objective] To optimize inclusion process for celery seeds oil with hydroxypropyl-β-cyclodextrin (HP-β-CD). Inclusion compound was also characterized and evaluated.[Methods] Inclusion complex was prepared by freeze-drying. Inclusion ratio,yield,contents of butylphthalide were the evaluated,and comprehensive score value was calculated. Inclusion temperature,inclusion time and feed ratio were investigated by single factor and three-factor five-level central composite design. The results were fitted by second or three-order polynomial multi-linear formulation. The predicted inclusion process was certificated to be optimal. Inclusion complex was determined by HPLC,UV and DSC.[Results] The optimal inclusion temperature was 44.5℃,the inclusion time was 167 min,and feed ratio of celery seed oil and HP-β-CD was 2:25. Inclusion rate of volatile oil was 78.95%,and the content of butylphthalide in complex was 2.982 mg/g. Characterization results showed that celery seed oil was successfully encapsulated by HP-β-CD.[Conclusion] The central composite design-response surface methodology was suitable to optimize the inclusion process. The mathematical model showed good predictability.