[关键词]
[摘要]
目的 研究右旋龙脑-β-环糊精最佳包合工艺,并对其进行结构表征。方法 分别采用饱和水溶液法、超声法、研磨法对右旋龙脑进行包合,以综合评分为指标,筛选最佳包合方法。采用L9(34)正交试验设计,筛选超声法制备包合物的最佳工艺参数。采用薄层色谱(TLC)法、傅里叶红外光谱(FIIR)法、X射线粉末衍射(XRD)法对包合物进行结构表征。结果 制备包合物的最佳工艺参数为:右旋龙脑与β-环糊精投料比为1∶6,超声温度为40 ℃,超声时间为60 min。在该制备工艺条件下包合物的得率高于88.59%,包合率高于95.98%。经过TLC、FIIR和XRD确证其包合物已形成。结论 本工艺具有较好的包合率和得率,右旋龙脑被β-环糊精包合后呈现新的物相特征。
[Key word]
[Abstract]
Objective To study the best preparation conditions of d-borneol-β-cyclodextrin inclusion complex and its structure characterization. Method The inclusion complex was prepared by the methods of saturated solution method, ultrasonic method, and grinding method with composite grade as index. To obtain the best preparation conditions of inclusion complex, L9(34) orthogonal test design was carried out. The structure of inclusion complex was identified by the methods of thin layer chromatography (TLC), Fourier infrared spectrum (FIIR) and X-ray powder diffractometry (XRD). Results The optimum preparation conditions were as follows: ratio of d-borneol and β-cyclodextrin was 1:6, ultrasound temperature was 40 ℃, ultrasound time was 60 min. The yield of inclusion complex was over 88.59%, and the inclusion ratio of inclusion complex was over 95.98% under the optimum conditions. The formation of inclusion complex was proved by TLC, FIIR, and XRD. Conclusion This technology has good inclusion rate and yield, and the d-borneol-β-cyclodextrin inclusion complex exhibits some new physical characteristics.
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[基金项目]
广东省自然科学基金博士启动项目(10451064101005160);省部产学研结合项目(2009A090100041,2010B090500033);中央高校基本科研业务费专项资金资助项目(2011ZM0099)