SU1223911A1 - Method of obtaining glyciram - Google Patents

Description

The invention relates to the pharmaceutical industry and can be used to obtain glycyram from licorice roots.

The purpose of the invention is to increase the yield of the final product and simplify the method. . Example. 200 g of crushed licorice root containing glycyrrhizic acid B., determined by a spectrophotometric method, are percolated in a l / o-HbiM diffuser with an aqueous M solution of ammonia until there is no qualitative reaction to glycerolic acid with methyl violet. The resulting extract is concentrated under vacuum to a volume equal to the weight of the taken root — about 200 ml. The condensed extraction is transferred to a vessel with a grinder and 95% ethanol is added, stirred. Ethanol is poured to its concentration in the extraction. .

The mixture is stirred for 15 minutes, the agitator is turned off and the mixture is left to stand at 5-8 ° C for 12 hours. Then the precipitate is filtered and washed on the filter with 55% ethanol. The filtrate and the washing alcohol are combined and, with stirring, poured into 95 ° / o-n M ethanol, bringing its concentration in the mixture to 89-91%. The resulting precipitate in the amount of 29.1 g with 46.37% glycyrrhizic acid content, determined by a spectrophotometric method, is filtered on a vacuum filter. The precipitate is dissolved in 3-5 volumes of water (100 ml) and passed through a column 2 cm in diameter with a layer of epoxy-polyamide anionite AB-16 G in hydroxyl form.

The grain size of the anion exchanger is 0.15-0.25 mm, the feed rate of the solution is 1.3-

1.5 ml min / cm, anion exchanger volume 20 ml. The passage through aionite is carried out until it is fully saturated with glycyrrhizic acid. The saturation completeness is determined by the concentration of the effluent solution, which, when complete saturation is reached, must be equal to the concentration of the incoming solution. The analysis is carried out by a spectrophotometric method. Acionite is washed with water and glycyrrhizic acid is desorbed with 4-6% aqueous ammonia solution, passing it through an anion exchanger at a rate of 1.0-1.2 ml min / cm2 (400 ml). The end of elution is determined by qualitative reaction with methylviolet. The eluate is evaporated and a dry residue of 2.2 g with a glycyrrhizic acid content of 69.9% is dissolved in ten volumes of 20% ethanol (20 ml), 3 ml of the swollen carboxyl cation exchanger KB-4P are added to the solution. -2 in H form. The cation exchanger and the solution is stirred for 30 minutes, the solution is filtered, the cation resin is washed with 5 ml of 20% alcohol. The solvent is evaporated, the content of glycyram in the residue (2.1 g) was 73.8%. The selection of the target product was carried out by crystallization from 90% alcohol, as a result of which the target product was obtained with a glycyrrhizic acid monoammonium salt content of 93.1%. The yield from glycyrrhizic acid sorbed by the anionite is 90%, in terms of the content in the raw material, the yield is 67.30 / 0.

According to the proposed method, the yield of glycyram is from 64 to 69%, and in the prototype 29%.

Claims (1)

METHOD FOR PRODUCING GLYCYRAM by extracting licorice roots with ammonia solution, precipitating glycyrrhizic acid, purifying and then isolating the target product by recrystallization from alcohol, characterized in that, in order to increase the yield of the final product and simplify the method, glycyrrhizic acid is precipitated from the extract with ethanol to the final concentrations of 54–56% are dissolved in water, and purification is carried out by sorption of it from a solution on anion exchange resin in hydroxyl form, desorption of a 4–6% aqueous solution of ammonia, and the resulting eluant evaporated to a dry residue was dissolved in 20 ° / o-prefecture ethanol and treated with carboxyl cationite in hydrogen form.