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款冬花活性化学成分分离及款冬酮提取工艺研究
Separation and Extraction Technology of chemical constituents from Tussilago farfara L
【Author】 CAO Kun~1,XU Yi~(*1,2,3) (1.Chemistry and Chemical Engineering College;Chongqing University,Chongqing,400030, P.R.China;2.Chongqing Strategic Alliance of Industrial Technology Innovation for New Drugs Innovation and Development;3.International R & D center of Micro-Nano Systems and New Materials Technology,Chongqing Univ.Chongqing China,400030)
【机构】 重庆大学化学化工学院;
【摘要】 款冬化是菊科植物款冬的干燥花蕾,主要成分是萜类、黄酮、生物碱和挥发油等,是一种传统中药。研究发现款冬花醇提物的石汕醚萃取层、乙酸乙酯萃取层具有升高血压、祛痰和抗炎等功效,且植物中的有效成分大都集中于此。实验以重庆道地药材款冬花为研究对象,采用传统的溶剂提取法,通过硅胶柱层析、TLC制备等过程,对款冬化醇提取物的石汕醚萃取层、乙酸乙酯苇取层浸膏进行系统分离,得到款冬酮、2,2-二甲基-6-乙酰基苯并二氢吡喃酮、金丝桃苷、芦丁、槲皮素和山奈酚等6种具有药用价值的单体化合物。款冬酮是款冬花中特有成分及药效成分,也是款冬花药材质量控制的标示性成分,研究其最佳提取工艺,提高提取效率,对款冬花的质量控制和进一步开发利用有重要的研究意义,但目前针对款冬酮的提取和分离纯化的相关研究较少。据此,提出以款冬酮得率为评价标准,考察了在同流提取法与超声提取法下,不同提取溶剂、提取时间、料液比对款冬酮提取效率的影响(表1),通过正交实验确定最佳提取条件,具体为:以50%甲醇为提取溶剂,料液比1:20,超声提取时间60min,款冬酮的得率达到1.53‰;与按药典[2010版]提取方法测定的款冬酮得率1.28‰相比,款冬酮得率提高18.8%。实验研究显示,所提出的提供方法重现性好、快捷高效,为款冬花中有效成分款冬酮的工业化提取及质量控制提供了物质基础和实验依据。
【Abstract】 The flower buds of Tussilago farfara L.was called as "Kuan Donghua" in China.It contained terpenoids,flavonoids,alkaloids and other phytochemicals,and was also known well as traditional Chinese medicine.It was shown that the extracts of petroleum ether(PE) and ethyl acetate(EtOAc) of the EtOH exaction of Tussilago farfara L.contained many active constitutions and has been used for the treatment of cough,bronchitis,and asthmatic disorders.In this paper,Tussilago farfara L which was one of genuine Chinese herb medicines in Chongqing area was proposed to be researched.The extract of PE and EtOAc were continually separated by various column chromatographic methods.Six compounds were obtained and structurally elucidated by NMR and MS.Those purified medicinal value compounds were tussilagone,2,2-Dimethyl-6-acetylchromanone,hyperoside,rutin,quercetin and kaempferol,respectively. Tussilagone,the significant phannacodynamic ingredient in the flower buds of Tussilagofarfara L.,was also the labeled component for quality control of the Tussilagofarfara L..It was concerned how to improve its extraction conditions and to increase its extracting efficiency,which undoubtedly has important implications for getting the utmost out of the flower buds of Tussihagofarfara L. However,so far,extraction and separation of Tussilagone has not been paid full attention to yet.In view of the above,thenno-refluxing method and ultrasonic wave method were put to work searching for more productive extraction.During the extracting process,three main factors including the ratio of solid to solvent,exacting time and solvent were investigated by using the orthogonal experiments design(L9(3+)),and the results were shown in Tab.1.Finally,the optimum conditions of ultrasonic extraction were obtained as follows:50%ethanol as extraction solvent for 60min,the ratio of solid to solvent was 1:20.Under these conditions,the yield oftussilagone was 1.53%o,which increased 18.8% more than extracted by the method in Chinese Pharmacopeia(2010 edition).The results also indicated that the proposed ultrasonic extracting method was of excellent reproducibility and accessibility. Absolutely,this method will play an active role in the dexelopment of industrial preparation of Tussilagone fiom Tussilagofarfara L..
【Key words】 Tussilago farfara L.; active chemical constituents; tussilagone; Ultrasonic Extraction;
- 【会议录名称】 化学与创新药物——2013年中国化学会产学研合作研讨会会议论文集
- 【会议名称】化学与创新药物——2013年中国化学会产学研合作研讨会
- 【会议时间】2013-10-16
- 【会议地点】中国重庆
- 【分类号】TQ461
- 【主办单位】中国化学会产学研合作与促进委员会、重庆市科学技术委员会