A kind of preparation method of 18α type glycyrrhizic acid diammonium salt

Abstract

The invention discloses a preparation method of 18 alpha type diammonium glycyrrhizinate. Under a certain alkali concentration, 18 beta type diammonium glycyrrhizinate is converted into 18 alpha type diammonium glycyrrhizinate. The end point is judged according to a principle that under a certain chromatographic condition, the retention time of 18 beta type diammonium glycyrrhizinate and the retention time of 18 alpha type diammonium glycyrrhizinate are different, and high performance liquid chromatography (HPLC) is used to judge the end point. The obtained 18 alpha type diammonium glycyrrhizinate is added into stronger ammonia water, and after refinement, qualified diammonium salt can be obtained. Compared with the conventional technology, the reaction temperature is reduced by about 10 DEG C, the time is also shortened, thus the energy loss of industrial production can be largely reduced; at the same time, the service life of equipment is prolonged, and the cost is reduced. Furthermore, the high temperature of conventional technology will deepen the product color, and the post treatment becomes difficult. The prepared 18 alpha type diammonium glycyrrhizinate has the advantages of good color, high yield and high content. The preparation method is suitable for industrial massive production, the product color is good, the crystals are uniform, and the quality is good.

Description

technical field [0001] The invention relates to the field of compound preparation, in particular to a preparation method of 18α-type diammonium glycyrrhizinate. Background technique [0002] Glycyrrhizic acid is the main component of natural medicine licorice. The structure is shown in the figure below (18β-type glycyrrhizic acid). It is an oleanane-type triterpene saponin compound, in which the 18-position carbon atom is a chiral carbon, and the compound is divided into 18α-type and 18β-type Type two configurations, in which 18β-type glycyrrhizic acid is the main component of licorice, while 18α-type glycyrrhizic acid only contains a very small amount. [0003] [0004] A large number of clinical experiments have shown that glycyrrhizic acid drugs have a wide range of pharmacological activities, such as activating or inhibiting enzyme activity, regulating substance metabolism, and regulating the excitability of cholinergic nerves. It has an obvious effect on convulsions...

AI Technical Summary

Problems solved by technology

[0005] 18α-type and 18β-type glycyrrhizic acid are epimer compounds. Since the content of 18α-type glycyrrhizic acid in plants is very small, it is not realistic to obtain it directly from plants. The configuration of type glycyrrhizic acid is relatively very stable, and it needs to be converted into 18α type glycyrrhizic acid under relatively harsh conditions. Generally, the conversion occurs under conditions of strong acid or strong alkali and high temperature (above 90°C), and the reaction time is usually For more than 30 hours, the judgment of the reaction end point is based on the maximum absorption wavelength of the product. In this case, the equipment requirements are relatively high. Moreover, the judgment method of the reaction end point cannot well explain the degree of configuration transformation.

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