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Preparation method of glycyrrhizic acid

A technology of glycyrrhizic acid and glycyrrhizic acid monoammonium salt, which is applied in the direction of steroids and organic chemistry, can solve the problems of long production process period of glycyrrhizic acid, low product yield, and many impurities, and achieve high production safety and high yield. The effect of high efficiency and high purity

Active Publication Date: 2017-09-01
JIANGSU TIANSHENG PHARMA
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  • Abstract
  • Description
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Problems solved by technology

[0004] Purpose of the invention: the present invention provides a preparation method of glycyrrhizic acid, which solves the problems of long production process cycle, many impurities, low purity and low product yield of glycyrrhizic acid

Method used

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  • Preparation method of glycyrrhizic acid
  • Preparation method of glycyrrhizic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Embodiment 1: get pulverized back and sieve (60-80 order) back glycyrrhizic acid coarse powder 100g, add the 80% ethanol of 800ml, extract 2 hours at 30 ℃ of temperature, obtain extract, 3g ammonium acetate is added extract, Add 0.1 g of formic acid, continue to stir for 0.5-1 h, transfer to room temperature for stirring and crystallization, and filter after 4 hours to obtain the crude product of monoammonium glycyrrhizinate. Get the crude product of monoammonium glycyrrhizic acid salt, add model is D001 strongly acidic cationic resin 20g, add 80% methyl alcohol of 20ml in the resin and carry out conversion under room temperature condition, obtain glycyrrhizic acid solution after conversion is completed, add 3g gradually at 30 DEG C ammonium acetate and 0.1g of formic acid, continuously stirred for 0.5-1h, transferred to room temperature for stirring and crystallization, filtered after 4 hours, and dried at 70°C for 5h to obtain 25.11g of monoammonium glycyrrhizinate, th...

Embodiment 2

[0040]Embodiment 2: get pulverized back and sieve (60-80 mesh) back glycyrrhizic acid coarse powder 100g, add the 95% ethanol of 1000ml and extract at 45 ℃ of temperature for 3 hours, extract solution adds the ammonium acetate of 8g and 2g at the same temperature The formic acid solution was continuously stirred for 0.5-1h, transferred to room temperature for stirring and crystallization, and filtered after 4 hours to obtain the crude product of monoammonium glycyrrhizinate. The test results of the crude monoammonium glycyrrhizinate are shown in Table 1. Get the monoammonium glycyrrhizinate crude product of gained glycyrrhizinate, add the strongly acidic cationic resin 50g that model is D001, add the 90% ethanol of 100ml and carry out conversion under the room temperature condition, obtain glycyrrhizic acid solution after conversion is completed, add the ammonium acetate of 8g and 2g of formic acid solution, continuously stirred for 0.5-1h, transferred to room temperature for s...

Embodiment 3

[0042] Embodiment 3: after getting crushed and sieved (60-80 order), glycyrrhizic acid coarse powder 100g, add the 90% ethanol of 1200ml and extract at 35 ℃ of temperature for 3 hours, extract solution adds the ammonium formate of 10g and 5g at the same temperature After stirring for a while, the acetic acid solution was transferred to room temperature for stirring and crystallization, and filtered after 4 hours to obtain the crude product of monoammonium glycyrrhizinate. Get the crude product of monoammonium glycyrrhizic acid salt, add the strong acid cationic resin 40g that model is LSI-010, add the 95% ethanol of 80ml and carry out conversion under the room temperature condition, obtain glycyrrhizic acid solution after conversion is completed, add the formic acid of 10g at 35 ℃ Ammonium and 5g of acetic acid solution, after stirring for a period of time, transferred to room temperature for stirring and crystallization, filtered after 4 hours, and dried at 70°C for 5h to obta...

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Abstract

The invention discloses a preparation method of glycyrrhizic acid. The preparation method comprises the following steps: firstly, adding glycyrrhizic acid crude powder into an ethanol solution for extracting, adding an extracting solution into an ammoniating solution, stirring, crystallizing and filtering; secondly, carrying out ion exchange on an obtained mono-ammonium glycyrrhizinate crude product in strong acidic cation resin to obtain a glycyrrhizic acid solution, adding the ammoniating solution into the glycyrrhizic acid solution, and stirring, crystallizing and filtering to obtain mono-ammonium glycyrrhizinate; thirdly, adding water into the mono-ammonium glycyrrhizinate for dissolving, and acidizing and filtering to obtain a glycyrrhizic acid solid; fourthly, dissolving the glycyrrhizic acid solid with an alkaline solution, diluting, absorbing with macroporous adsorption resin, eluting and collecting eluant; fifthly, transforming the eluant by using strong acid cation exchange resin, and removing a solvent of a transformation solution to obtain glycyrrhizic acid powder. The preparation method disclosed by the invention has the advantages of short process period, low cost and high safety; the obtained product has the characteristics of high yield, good color and high purity. The glycyrrhizic acid prepared by the preparation method disclosed by the invention can be applied to the fields of medicine and food.

Description

technical field [0001] The invention belongs to a preparation method of plant medicinal components, in particular to a preparation method of glycyrrhizic acid. Background technique [0002] Glyrrhizic acid (Glyrrhizic acid), also known as glycyrrhizin and glycyrrhizin, is a triterpene saponin extracted from the dried roots and rhizomes of Glycyrrhizauralensis fisch. It is a white or light yellow crystalline powder with a melting point of 220°C and a special sweet taste. Molecular formula: C 42 h 62 o 16 , Molecular weight: 822.92. Glycyrrhizic acid in nature exists in two configurations of α-body and β-body, and the content of α-body is lower than 5% of β-body. The melting points of the two isomorphic crystals are 300-304°C and 287-293°C respectively, easily soluble in hot water and ethanol, and almost insoluble in ether. Glycine aminotransferase, restore liver cell function, prevent fatty change, promote bile pigment metabolism, jaundice and detoxification, reduce coll...

Claims

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Application Information

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IPC IPC(8): C07J63/00
CPCC07J63/008
Inventor 季浩张宇阚建伟于燕燕刘佳窦长清孔繁博徐娟
Owner JIANGSU TIANSHENG PHARMA
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