星点设计-效应面法优化鱼腥草挥发油-β-环糊精包合物的制备工艺

Optimization of preparation of volatile oil from Houttuynie Herba-β-cyclodextrin inclusion complex by central composite design-response surface method

目的优化鱼腥草挥发油-β-环糊精(β-CD)包合物的制备工艺。方法采用搅拌法制备包合物,以挥发油包合率、包合物得率和包合物中甲基正壬酮质量分数的综合评分OD值为评价指标,在单因素试验基础上采用3因素5水平星点设计考察包合时间、包合温度、β-CD与鱼腥草挥发油投料比对制备工艺的影响,对结果进行多元线性和二项式拟合,效应面法筛选出最佳包合工艺,进行预测分析和验证试验,并以红外光谱法和顶空固相微萃取-气相色谱-质谱法(HS-SPME-GC-MS)对包合物进行质量评价。结果鱼腥草挥发油-β-CD包合物的最优包合工艺:包合时间4.8 h、包合温度62℃、β-CD与鱼腥草挥发油的质量比为7.79∶1,挥发油包合率、包合物得率和包合物中甲基正壬酮质量分数预测值与理论值的偏差分别为1.70%、1.49%、2.22%。结论星点设计-效应面法适用于鱼腥草挥发油-β-CD包合物的制备工艺优化,以此方法建立的数学模型具有良好的预测性。

Objective To optimize the preparation process of volatile oil prepared from the aerial parts of Houttuynia cordata（Houttuynie Herba,HH）-β-cyclodextrin（β-CD） inclusion complex by central composite design-response surface method.Methods To prepare the inclusion complex by stiring,with the overall desirability（OD） values of inclusion ratio,yield of the inclusion complex,and methyl-n-nonyl-ketone content as indexes,the influence of inclusion temperature,inclusion time,and ratio of β-CD-HH volatile-oil to inclusion process was investigated by response surface method,the results were fitted by multi-linear equation and second-order polynomial equation,and the optimal inclusion process was predicted according to formulation.The quality of inclusion complex was evaluated by IR and HS-SPME-GC-MS.Results The optimal inclusion technologies of the HH volatile oil-β-CD inclusion complex were as follows：inclusion time 4.8 h,inclusion temperature 62 ℃,and ratio of β-CD-HH volatilel oil 7.79∶1.Bias of inclusion ratio,yield of the inclusion complex,and methyl-n-nonyl-ketone content between observed and predicted values were 1.70%,1.49%,and 2.22% respectively.Conclusion Using the central composite design-response surface method to optimize the preparation of HH volatile oil-β-CD inclusion complex has a good prediction.