目的 制备降香油-羟丙基-β-环糊精包合物并对其工艺进行优化。方法 采用搅拌-冷冻干燥法制备降香油-羟丙基-β-环糊精包合物,以包合物收率、挥发油利用率及反式-橙花叔醇含量的综合评分为评价指标,使用星点设计-效应面法进行工艺优化;采用相溶解度法、差示扫描量热法、紫外扫描法及显微鉴定对包合物进行鉴别。结果 降香油-羟丙基-β-环糊精包合物的最佳制备工艺为:以体积分数5%乙醇为包合溶媒,搅拌速度500 r·min-1,主客体投料比33∶1,包合温度42 ℃,包合时间2.5 h。包合物的形成会导致主客体分子的溶解度、光学及热力学性质发生变化,可作为鉴别的依据。结论 采用星点设计-效应面法优化所得降香油-羟丙基-β-环糊精包合物的制备工艺合理可行,为降香油的进一步开发利用提供了依据。
Abstract
OBJECTIVE To prepare the inclusion complex of Lignum dalbergia odorifera oil with hydroxyl-β-cyclodextrin(HP-β-CD), and to optimize the preparation process of it. METHODS The inclusion complex was prepared by the stirring-freeze-dry method. The preparation process was optimized by central composite design-response surface method (CCD-RSM),with the colligation score which was calculated by the yield of inclusion, the utilization rate of volatile oil and the content of trans-nerolidol as index. The inclusion complex was verified by phase-solubility method, DSC,UV and microscopical identification. RESULTS The optimum inclusion technology was: inclusion solvent 5% ethanol, stirring rate 500 r·min-1, HP-β-CD to volatile oil 33∶1, inclusion temperature 42 ℃,inclusion time 2.5 h. The formation of inclusion complex can change the solubility, optical and thermodynamic properties of volatile oil. CONCLUSION The preparation process of inclusion complex of Lignum dalbergia odorifera oil with HP-β-CD optimized by CCD-RSM is reasonable and feasible, and provide a reliable experiment basis for its application.
关键词
降香油 /
羟丙基-β-环糊精 /
星点设计-效应面法 /
包合物 /
制备工艺
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Key words
Lignum dalbergia odorifera oil /
hydroxypropyl-β-cyclodextrin /
central composite design-response surface method(CCD-RSM) /
inclusion complex /
preparation process
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中图分类号：
R944
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参考文献
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脚注
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基金
国家“重大新药创制”科技重大专项课题(2009ZX09310-002)
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