离子液体/盐双水相体系萃取分离葛根素研究
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摘要
葛根含有丰富的药理活性成分,其临床应用前景相当乐观,具有很高的开发价值。本文就葛根中的葛根素进行了提取分离研究,建立了离子液体/盐双水相体系萃取葛根素的新方法,并借助高效液相手段定量分析,为葛根的开发利用提供了科学依据。具体的研究内容和结论如下:
     合成一系列不同的离子液体,在离子液体上引入各种功能基,使之与葛根素具有较独特的作用,以便筛选出合适的离子液体。
     基于离子液体/盐的双水相体系相图的绘制,筛选出能够稳定成相,以及萃取葛根素时具有良好的萃取率和选择性的双水相体系。考察离子液体、盐种类及量的变化等因素对双水相体系成相及对葛根素萃取率的影响。
     结合[Bmim]Br/K2HPO4双水相体系和超声辅助萃取法对粗葛根进行萃取,考察葛根量、超声功率及超声时间等对提取率的影响,并且和常规方法比较显示该方法的优越性。结合响应面法设计实验,探索适合提取葛根中葛根素的工艺条件为:系统总体积设计为5m1,在36%(g/ml)[Bmim]Br/30%(g/ml)K2HPO4双水相体系中,葛根加入量为0.3g,超声功率420W,超声温度35℃,提取时间15min,在上述提取条件下,提取率可达87.91%。
     比较不同的离子液体水溶液与超声辅助法直接提取葛根素。由于离子液体的阴阳离子不同,对葛根素的提取效果有明显的区别,分析筛选出最佳的离子液体进行条件的优化。结合响应面法设计实验,得到最佳工艺条件为:系统总体积设计为10ml,在1.0mol/l的[Bmim]Br水溶液中加入0.5g葛根粉末,35℃、480W超声提取30min得到最大的提取率82.23%。
Pueraria is rich in pharmacologically active ingredient, it is quite optimistic in the clinical application. This article is about the extraction separation of puerarin in pueraria, the ionic liquid/salt aqueous two-phase extraction systems were studied and the content of puerarin is measured using high performance liquid chromatography.It provides a scientific basis for the development and utilization of Pueraria. The main research contents and conclusion were as follows:
     A series of different ionic liquids and introduce a variety of functional groups in ionic liquids were synthesized, in order to select the best ionic liquid which has a unique interaction with puerarin.
     Through constructing the ionic liquid/salt aqueous two-phase system phase diagrams, the two-phase system can be selected with stable two-phase, and the good extraction rate and the high selectivity of. puerarin. Experimental conditions of the system have been optimized, including the amount and types of ionic liquid, salt and other factors on the phase behavior and extraction rate of puerarin.
     Ultrasonic-assisted, ionic liquid-based aqueous two-phase system was investigated to obtain effective constituent, puerarin in pueraria. The procedure was also optimized on some parameters, such as the amount of pueraria, salt, ionic liquid, ultrasonic power and ultrasonic time. And compared with conventional methods,it shows the superiority of the method. Response surface experimental design was used to explore for the best extraction conditions of puerarin in Pueraria:The total volume was designed to 5ml, in the 36%(g/ml)[Bmim]Br/30%(g/ml)K2HPO4 system, the amount of pueraria 0.3g,ultrasonic power 420W,ultasonic temperature 35℃, etraction time 15min.The yield of puerarin was 87.91%.
     Comparing the ultrasonic assisted extraction methods by different ionic liquids with different cations and anions, it was significantly different on the extraction rate of puerarin, and then the optimal conditions for ultrasonic assisted extraction of puerarin in pueraria were studied. Response surface experimental design was used to explore for the best extraction conditions of puerarin in Pueraria:The total volume was designed to 10ml,in the [Bmim]Br solution of 1.0mol/l,the amount of pueraria 0.5g,ultrasonic power 480W,ultasonic temperature 35℃, etraction time 30min.The yield of puerarin was 82.23%.
引文
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