丹参活性部位丹参二萜醌羟丙基-β-环糊精包合物的制备工艺研究

Preparation technology of diterpenoid tanshinone hydroxypropyl-β-cyclodextrin inclusion complex from active parts of Salvia miltiorrhiza

目的优化丹参二萜醌(diterpenoid tanshinone,DT)羟丙基-β-环糊精(hydroxypropyl-β-cyclodextrin,HP-β-CD)包合物(inclusion complex,IC)(DT&HP-β-CD@IC)制备工艺。方法在单因素试验的基础上,选择DT与HP-β-CD的配比、包合温度、包合时间为考察因素,以DT包封率及包合物载药量为综合评价指标,利用Box-Behnken响应面优化DT&HP-β-CD@IC制备工艺,并采用红外光谱法、紫外光谱法、薄层色谱法及扫描电子显微镜法对DT&HP-β-CD@IC进行评价。结果DT&HP-β-CD@IC最佳制备工艺为HP-β-CD质量浓度0.1 g/mL,药物与载体材料配比1∶3,包合时间2 h,包合温度40℃。DT&HP-β-CD@IC的包封率达68.78%,载药量达5.44%。紫外、红外光谱和薄层色谱等结果表明DT&HP-β-CD@IC的形成。结论DT&HP-β-CD@IC载药量较高,溶解性有一定的提高。

Objective To optimize the preparation process of diterpenoid tanshinone(DT)hydroxypropyl-β-cyclodextrin(HP-β-CD)inclusion complex(IC)(DT&HP-β-CD@IC).Methods Based on the single factor test,the ratio of DT and HP-β-CD,the inclusion temperature,and the inclusion time were selected as the investigating factors,the encapsulation efficiency and drug-loading of the inclusion complex were used as the evaluation index.The Box-Behnken response surface was used to optimize the preparation process of the DT&HP-β-CD@IC,and the inclusion complex was evaluated by infrared spectroscopy,ultraviolet spectroscopy,thin layer chromatography and scanning electron microscopy.Results The optimal preparation process of the inclusion complex was as follows:HP-β-CD concentration was 0.1 g/mL,the ratio of drug to carrier material was 1:3,the inclusion time was 2 h,and the inclusion temperature was 40℃.The encapsulation rate of DT&HP-β-CD@IC was 68.78%,and the drug loading was 5.44%.The results of ultraviolet,infrared spectroscopy and thin-layer chromatography indicated the formation of inclusion complex.Conclusion DT&HPβ-CD@IC has a high encapsulation efficiency and a certain improvement in solubility.