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Preparation method of monoammonium glycyrrhizinate

A technology of glycyrrhizic acid monoammonium salt and glycyrrhizic acid is applied in the directions of steroids, organic chemistry, etc., can solve the problems of complex method, low yield, insufficient purity of finished products, etc., and achieves simplified preparation process, high purity and yield, The effect of reducing the generation of alkali-soluble impurities

Active Publication Date: 2017-03-08
QINGHAI LAKE PHARMA COMPANY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the prior art, the preparation and purification process of monoammonium glycyrrhizinate mostly adopts the method of water boiling, alcohol precipitation and extraction combined with multiple crystallization and purification, which is not only complicated, but also the purity of the finished product is not enough, and the yield is low

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  • Preparation method of monoammonium glycyrrhizinate

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preparation example Construction

[0025] The invention provides a kind of preparation method of monoammonium glycyrrhizinate, comprising:

[0026] A) extracting licorice with an organic solvent, acid precipitation, and obtaining crude glycyrrhizic acid;

[0027] B) extracting the crude product glycyrrhizic acid with an organic solvent, decolorizing and ammoniating to obtain an ammoniated solution;

[0028] C) ultrafiltering the ammoniated solution to obtain monoammonium glycyrrhizinate.

[0029] In the invention, firstly, the licorice is extracted with an organic solvent and acid-precipitated to obtain crude glycyrrhizic acid. In the present invention, firstly, the licorice is extracted with an organic solvent. The licorice in the present invention is preferably extracted after being pulverized. The method of pulverization is not limited in the present invention, it can be pulverized into grass silk, and the pulverization method well known to those skilled in the art can be used. The organic solvent is pref...

Embodiment 1

[0066] Weigh 200g of crushed licorice, add 1.6L of 91% ethanol, ultrasonically extract at 60°C for 1h, and filter; The pH was 2.1, and 20.0 g of crude glycyrrhizic acid was obtained. Through measurement and calculation, the extraction rate of glycyrrhizic acid was 92.8%, and the content of glycyrrhizic acid in the crude glycyrrhizic acid was 31.2%.

[0067] The crude glycyrrhizic acid was extracted twice with 150 ml of 91% ethanol. After the ethanol extract was decolorized with activated carbon, ammonia water was added to adjust the pH value to 4.8, and ammoniated to obtain an ammoniated solution.

[0068] The ammoniated solution is ultrafiltered with a polyethersulfone ultrafiltration membrane with a molecular weight cut-off of 2500-3000. The temperature is 30°C, the pressure is 0.05Mpa, and the feed concentration is 30g / L. The filtrate is crystallized, filtered, dried, and pulverized to obtain the product . Using ultraviolet absorption spectroscopy, infrared absorption spec...

Embodiment 2

[0070] Weigh 200 g of crushed licorice, add 2.0 L of acetone, ultrasonically extract at 50 ° C for 1 h, and filter; add 2.0 L of acetone to the filter residue, ultrasonically extract at 50 ° C for 1 h, filter, combine the filtrates, and use 5% hydrochloric acid to precipitate until the pH is 1.9, to obtain Crude glycyrrhizic acid is 19.8g, the extraction rate of glycyrrhizic acid is 90.5%, and the content of glycyrrhizic acid in crude glycyrrhizic acid is 30.5%.

[0071] The crude glycyrrhizic acid was extracted twice with 160 mL of 93% ethanol. After the ethanol extract was decolorized with activated carbon, ammonia water was added to adjust the pH value to 5.0, and ammoniated to obtain an ammoniated solution.

[0072] The ammoniated liquid is subjected to membrane ultrafiltration using a polyethersulfone ultrafiltration membrane with a molecular weight cut-off of 2500-3000. The temperature is 30°C, the pressure is 0.10Mpa, and the feed concentration is 40g / L. The filtrate is ...

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Abstract

The invention provides a preparation method of monoammonium glycyrrhizinate. The method comprises steps as follows: A) glycyrrhiza uralensis is subjected to extraction with an organic solvent and acid precipitation, and a crude glycyrrhizic acid product is obtained; B) crude glycyrrhizic acid product is subjected to extraction with an organic solvent, decolorization and ammoniation, and an ammoniation liquid is obtained; C) the ammoniation liquid is subjected to ultrafiltration and monoammonium glycyrrhizinate is obtained. The method innovatively treats the glycyrrhiza uralensis in the organic solvent extraction and acid precipitation manner, compared with the prior art, the method can extract glycyrrhizic acid more effectively, and compared with an alkaline extraction manner, the method can reduce alkaline-soluble impurities. Monoammonium glycyrrhizinate can be directly produced after ammoniation, crystallization can be directly performed without acidification crystallization once again, the preparation process is simplified, and ultrafiltration extraction is combined, so that the purity and the yield of the prepared monoammonium glycyrrhizinate are high.

Description

technical field [0001] The invention relates to the technical field of compound preparation, in particular to a preparation method of monoammonium glycyrrhizinate. Background technique [0002] Monoammonium glycyrrhizinate is an important raw material for food, medicine and cosmetics, which is refined from planted licorice through extraction, acidification, ammonification, recrystallization and other processes. Its applications cover food, medicine, cosmetics, advanced Industries such as cigarettes and toothpaste. [0003] In the food industry, monoammonium glycyrrhizinate is mainly used as a sweetener. On the one hand, its sweetness is about 200 times that of sucrose; Moreover, it can also prevent some foods from easily fermenting, spoilage, deterioration, browning and solidification caused by a large amount of white sugar. In addition, it can increase the thickness of sweetness, present umami, reduce sourness and rawness. The role of fishy smell. The scope of applicatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
CPCC07J63/008
Inventor 骆俊才苏旺平胡建彪梁俊才
Owner QINGHAI LAKE PHARMA COMPANY
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