荆防颗粒挥发油β-环糊精制备工艺的优化

Optimization of preparation process of Jingfang volatile oilβ-cyclod-extrin

目的优化荆防颗粒挥发油β-环糊精包合物制备工艺。方法以挥发油包合率、包合物得率为评价指标,比较胶体磨法、饱和水溶液法、超声法包合物制备工艺,确定包合方法;在单因素实验的基础上,采用Box-Behnken响应面法,以挥发油包合率、包合物得率的综合评分为考察指标,考察挥发油与β-环糊精的比例(1∶6~1∶10)、β-环糊精与水的比例(1∶2~1∶4)以及研磨包合时间(15~25分钟)对包合物制备工艺的影响,通过气相色谱法对包合前后挥发油化学成分进行检测。结果经对比,胶体磨法得到的包合物挥发油包合率(80.37%)和包合物得率(86.55%)均高于饱和水溶液法(75.19%、79.49%)和超声法(68.38%、72.05%),故选择胶体磨法制备荆防颗粒挥发油β-环糊精包合物;优选出的最佳工艺条件为挥发油∶β-环糊精为1∶8,β-环糊精∶水为1∶3,研磨包合时间为21分钟,3次验证实验结果显示,挥发油包合率平均为85.98%,包合物得率平均为92.51%。结论优选的荆防颗粒挥发油包合工艺包合率和包合物得率均较高,包合工艺科学、合理、可行。

Objective To optimize the inclusion process of volatile oil wra-pped withβ-cyclodextrin in Jingfang granules.Methods Taking volatile oil inclusion rate and inclusion compound yield as evaluation indicators,the preparation process of inclusion compounds by colloid milling method,saturated aqueous solution method and ultrasonic method was compared,and the inclusion method was determined.On the basis of the single factor experiment,the Box-Behnken response surface method was used to investigate the ratio of volatile oil toβ-cyclodextrin(1∶6~1∶10),the ratio ofβ-cyclodextrin to water(1∶2~1∶4),and the grinding and inclusion time(15~25 min)on the preparation process of the inclusion compound.The volatile oil before and after inclusion was analyzed by gas chromatog-raphy.Chemical composition testing.Results The inclusion rate(80.37%)and the inclusion rate(86.55%)of the inclusion compound volatile oil obtained by the colloid milling method are higher than that obtained by the saturated aqueous solution method(75.19%,79.49%)and ultrasonic method(68.38%,72.05%),so the colloid milling method was chosen to prepare Jingfang volatile oilβ-cyclodextrin inclusion complex.The optimal inclusion process was as follows:the ratio of volatile oil toβ-cyclodextrin was 1∶8,the ratio ofβ-cyclodextrin to water was 1∶3,and the grinding inclusion time was 21 min.The results of 3 verification experiments show that the average inclusion rate of volatile oil is 85.98%,and the average yield of inclusion compound is 92.51%.Conclusion Using Box-Behnken response surface method to optimize the inclusion rate of Jingfang granule volatile oil inclusion rate and the inclusion rate of inclusion compound are both high,and the inclusion process is scientific,reasonable and feasible.