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A method for preparing high-purity glycyrrhizic acid

A high-purity glycyrrhizic acid technology, which is applied in the preparation of sugar derivatives, chemical instruments and methods, steroids, etc., can solve the problems of difficulty in obtaining high purity and low efficiency of glycyrrhizic acid, and achieve low cost and high product purity , cost reduction effect

Inactive Publication Date: 2011-12-21
XIAN RUILIAN NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods have their own advantages and disadvantages, using one of the methods to purify glycyrrhizic acid is less efficient or it is difficult to obtain high-purity products

Method used

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  • A method for preparing high-purity glycyrrhizic acid
  • A method for preparing high-purity glycyrrhizic acid
  • A method for preparing high-purity glycyrrhizic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0028] 1. Preparation of Monoammonium Glycyrrhizinate

[0029] Dissolve 100.0 g of crude product with a glycyrrhizic acid content of 10% in 700 ml of water, add dilute sulfuric acid under stirring to adjust its pH to 2.0, filter, and dry at room temperature to obtain crude glycyrrhizic acid. Add 6 times the amount of acetone to the crude glycyrrhizic acid and reflux for leaching for 2 hours, pass ammonia gas into the leaching solution to make the pH value 8.0-9.0, make it react to form triammonium glycyrrhizinate, filter, add to the precipitate 6 times the amount of glacial acetic acid to obtain the crude product of monoammonium glycyrrhizinate. The monoammonium glycyrrhizinate crude product is recrystallized, the solvent ratio is chloroform: ethanol: water = 1: 5: 5, the solid-liquid ratio is 1: 2, and the dissolution temperature is 70 ° C. After the temperature drops to room temperature, place it in an ice-water bath After 3 hours, filter, dry the crystalline product at 60°...

Embodiment 2

[0041] 1. Preparation of Monoammonium Glycyrrhizinate

[0042] Dissolve 100.0 g of the crude product with a glycyrrhizic acid content of 10% in 700 ml of water, add dilute sulfuric acid under stirring to adjust the pH to 3.0, filter, and dry at room temperature to obtain the crude glycyrrhizic acid. Add 6 times the amount of acetone to the crude glycyrrhizic acid and reflux for leaching for 2 hours, pass ammonia gas into the leaching solution to make the pH value 8.0-9.0, make it react to form triammonium glycyrrhizinate, filter, add to the precipitate 6 times the amount of glacial acetic acid to obtain the crude product of monoammonium glycyrrhizinate. The crude product of monoammonium glycyrrhizinate salt is recrystallized, the solvent ratio is chloroform: ethanol: water = 1: 4: 4, the solid-liquid ratio is 1: 2, and the dissolution temperature is 70 ° C. After the temperature drops to room temperature, place it in an ice-water bath After 4 hours, filter, dry the crystalliz...

Embodiment 3

[0052] 1. Preparation of Monoammonium Glycyrrhizinate

[0053] Dissolve 100.0 g of the crude product with a glycyrrhizic acid content of 10% in 700 ml of water, add dilute sulfuric acid under stirring to adjust its pH to 4.0, filter, and dry at room temperature to obtain crude glycyrrhizic acid. Add 6 times the amount of acetone to the crude glycyrrhizic acid and reflux for leaching for 2 hours, pass ammonia gas into the leaching solution to make the pH value 8.0-9.0, make it react to form triammonium glycyrrhizinate, filter, add to the precipitate 7 times the amount of glacial acetic acid to obtain the crude product of monoammonium glycyrrhizinate. The monoammonium glycyrrhizinate crude product is recrystallized, the solvent ratio is chloroform: ethanol: water = 1: 3: 3, the solid-liquid ratio is 1: 2, and the dissolution temperature is 70 ° C. After the temperature drops to room temperature, place it in an ice-water bath After 3 hours, filter, dry the crystalline product at...

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Abstract

The invention relates to a method for preparing high-purity glycyrrhizic acid, comprising the following steps: (1) preparation of monoammonium glycyrrhizic acid, (2) preparation of crude glycyrrhizic acid, (3) polyamide column chromatography to remove key impurities 1 , (4) recrystallization to remove key impurity 2, (5) polyamide purification of glycyrrhizic acid. The characteristics of the present invention are: the present invention prepares high-purity glycyrrhizic acid, the column chromatography is efficient and convenient, and the separation capacity is large, which is suitable for complex sample separation and purification; polyamide and cation exchange resin can be regenerated and reused by simple methods, reducing costs, The equipment used is simple and suitable for industrial production; high-purity glycyrrhizic acid can be obtained through polyamide adsorption column purification. It has the following advantages: high product purity, the content of glycyrrhizic acid reaches more than 99.5 percent; the cation exchange resin and polyamide can be reused, and the cost is low; the operation is simple; the equipment investment is small, the environment is friendly, and it is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of extraction of natural medicines, in particular to a method for preparing high-purity glycyrrhizic acid. Background technique [0002] Glycyrrhizic acid (Glycyrrhizic Acid), also known as glycyrrhizin, glycyrrhizin, molecular formula C 42 h 62 o 16 , the molecular weight is 822.92, and its structural formula is as follows: [0003] [0004] Glycyrrhizic acid is in the form of white crystalline powder, odorless, and has a special sweet taste. It is one of the most important active ingredients in licorice. In recent years, it has also been widely used in pharmaceutical, chemical, food, daily chemical and other industries. Clinically, it is widely used in the treatment of various acute and chronic hepatitis, bronchitis and AIDS. In addition, glycyrrhizic acid can also be anti-cancer and anti-cancer, an interferon-inducing agent and a cellular immune regulator. It has non-specific immunoregulatory effects, lower...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00C07H15/256C07H1/06
Inventor 邓师勇李启贵杨代兵强婷华冯震冯小琼
Owner XIAN RUILIAN NEW MATERIAL CO LTD
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