大黄游离蒽醌提取工艺的正交优化研究

Research on the Optimization of Rhubarbs Extraction Process Using Orthogonal Test

目的:从药材大黄中提取游离蒽醌类化合物并分离其各个组分,优选大黄游离蒽醌化合物的提取工艺。方法:酸处理大黄粗粉,使蒽醌苷脱糖链水解成为游离的羟基蒽醌,有机溶剂萃取得总游离蒽醌,pH梯度萃取依次分离并得到大黄酸、大黄素、芦荟大黄素、大黄酚和大黄素甲醚组分。正交试验法考察水解时间、回流时间、提取温度和提取溶剂对大黄总游离蒽醌及各组分提取效果的影响,对其产物进行分析。结果:以总蒽醌为指标,最佳提取条件为药材粗粉用20%硫酸微沸水解3小时,氯仿在99℃下回流提取4小时。以各个组分为指标,溶剂的主导影响因素更为明显,氯仿对各成分均有较好浸提效果;苯仅对大黄酚和大黄素甲醚效果好,石油醚对所有组分都不理想。结论:优化的最佳因素组合是稳定高效的提取工艺。

ObjectiveExtract total dissociated anthraquinones from rhubarbs and then separate every single component from the total dissociated anthraquinones, Optimize the Rhubarbs Extraction Process. MethodsCrude rhubarbs powder was disposed by acid, and the anthraquinone glycoside was hydrolyzed to the state of aglycone. Then it was extracted by organicsolvents, and thetotal dissociated anthraquinones were obtained. With pH value grades extraction method, every component was isolated, such as rhein, emodin, aloe -emodin, chrysophanol, physcion. Different hydrolyzing time, refluxing time, extracting temperature and extracting solvent were assayed by orthogonal test to detect their influences on the extraction rate of anthraquinone. ResultsIndicated by the total dissociated anthraquinones yield, the best condition was： using 20% sulfuric acidsolution hydrolyzed 3 h, reflux extracted 4 h at 99℃ with chloroform. Indicated by the yield of every component, extracting solvent was the dominantinflueneing factor, chloroform performenced well to every kind of component; benzene was only good for chrysophanol and physcion; petroleum ether was the worst extracting solvent. ConctusionThe optimal combinationof the influencing factors was an efficient extraction process.