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微波辅助提取甘草中有效成分的研究及甘草的综合利用
Microwave-Assisted Extraction of Useful-Component from Liquorice and Comprehensive Utilization of Glycyrrhiza
【作者】 阚微娜;
【导师】 谭天伟;
【作者基本信息】 北京化工大学 , 生物化工, 2006, 硕士
【摘要】 本文以分离纯化甘草中的主要有效成分甘草酸和甘草黄酮类化合物为目的,系统研究了利用微波提取技术(MAE)同时从甘草中提取主要有效成分,并通过后续的精制过程分别得到甘草酸和甘草黄酮的工艺。在前人实验研究的基础上,首先建立了甘草酸和甘草总黄酮类化合物的高效液相色谱和紫外—可见分光光度分析检测方法,作为在分离过程中检测目标产物的手段。通过单因素实验和正交设计实验,考察了提取溶剂、液固比、微波辐照时间、微波功率及甘草原料的粒度等因素对甘草有效成分提取的影响,并以甘草酸和甘草黄酮类化合物的提取率为指标,确定了微波辅助提取过程的最佳实验条件,即使用70%的乙醇水溶液,液固比为25:1,微波功率350w,提取温度60℃,对于20g甘草粉末微波辐照10min(总提取时间为30min),一次提取甘草酸的提取率可达到3.81%,甘草总黄酮提取率为4.40%。,与传统的热回流和索式提取法等相比,操作简便,大大缩短了提取的时间,减少了其他杂质的浸出率,节省了能源。甘草有效成分的精制工艺主要使用的是简单的溶剂提取,调节pH值沉淀等方法。同时采用正交设计实验,对精制工艺进行了优化,其中最佳酸性乙醇提取条件为:提取温度40℃,提取4h,提取溶剂为pH3~4的95%乙醇。最终得到纯度为96%以上的甘草酸单铵盐无色晶体及含量为40%左右的甘草黄酮类化合物,有效的对提取液中的甘草酸和甘草黄酮进行了分离,实现了甘草的综合利用。
【Abstract】 The purpose of this study was to develop an efficient process for isolation and purification of the useful-component from liquorice. Microwave-assisted extraction (MAE) method was studied for the extraction of glycyrrhizic acid (GA) and licoflavones from the roots of Glycyrrhiza species. And through the refining process, GA and licoflavones can be got separately.On base of studying of the other people, the methods of analyzing GA by HPLC and licoflavones by spectrophotomer were founded.Several factors, such as extraction solvent, time, liquid/solid ratios materials size and microwave power, which were effected MAE operation were investigated by single factor experiments and orthogonal experiments And the optimal conditions were obtained from the experiments. The optimum conditions of MAE is10min extracting in70%ethanol water solvent at60℃under the microwave heating, microwave power350W, and the liquid/solid ratios of25:1(mL/g). Under this condition, we can both extract glycyrrhizic acid (GA) and licoflavones efficiently. The extracting percentage of GA was3.81%, and the licoflavones was4.40%. Comparing with other traditional methods, such as hot reflux extraction and soxhlet extraction, MAE method is fast, efficient and energy saving, which is recommendable to the application to useful-component extraction form the Chinese traditional medicine.To separate GA and licoflavones only used some easy steps, for example, solvent extraction, pH value adjustment. Based on the results of orthogonal design, the best refining procedure is as follows:95%ethanol water solvent, pH=3-4, temperature40℃, time4h. At last, the colorless monoammonium glycyrrhizinate crystal with purity of96%and licoflavones with the content of40%were got.
【Key words】 microwave-assisted extraction; glycyrrhizic acid; licoflavones; purification;