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Method for preparing mono-ammonium glycyrrhizinate

A technology of glycyrrhizic acid monoammonium salt and glycyrrhizic acid powder is applied in the directions of steroids, organic chemistry, etc., can solve problems such as high production cost, low product content, complicated process, etc., and achieves easy operation, high product content, and cost reduction. Effect

Inactive Publication Date: 2009-09-02
XINJIANG FUWO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Glycyrrhizinate monoammonium salt is the third generation substitute of the active ingredient of traditional Chinese medicine licorice, and it has strong anti-inflammatory, liver cell membrane protection and liver function improvement effects. At present, the synthesis method of glycyrrhizinate monoammonium salt is generally prepared from licorice Glycyrrhizic acid powder, and first by synthesizing triammonium glycyrrhizinate, then adding acetic acid to prepare monoammonium glycyrrhizinate, the process is many, the process is complicated, the production cost is high, and needs to use a large amount of solvent, the solvent used is not conducive to environmental protection, and the product content obtained lower

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Example 1: Take 1Kg of glycyrrhizic acid powder, add 6Kg of 95% ethanol for the first time to reflux for extraction at 50°C for 2 hours, filter and then add 8Kg of 95% ethanol, reflux for 2 hours, filter, then add 6Kg of 95% ethanol, reflux for 2 hours, and combine Add ammonia gas to the above filtrate until the pH value is between 5 and 6, stir for 1 h, let it stand for 24 h, and filter with suction to obtain the crude product of monoammonium glycyrrhizinate. After the solution is clear, add 25g of activated carbon, reflux for extraction for 1 hour, pour it out, let it stand for 12 hours, filter it with suction, and dry it in vacuum until the water content is 8%, to obtain the finished product of monoammonium glycyrrhizinate.

Embodiment 2

[0010] Example 2: Take 1Kg of glycyrrhizic acid powder, add 8Kg of methanol for the first time to reflux for extraction at 50°C for 2h, filter and then add 5Kg of methanol, reflux for 2h, filter, then add 5Kg of methanol, reflux for 2h, combine the filtrates, and feed ammonia gas , until the pH value is between 5 and 6, stir for 1h, let stand for 24h, and suction filter to obtain the crude product of monoammonium glycyrrhizinate. Add 6Kg of 85% ethanol to dissolve the monoammonium glycyrrhizinate. After the solution is clear, add 30g of activated carbon. Reflux for extraction for 1 hour, let stand for 12 hours, filter with suction, and vacuum-dry until the water content reaches 6%, to obtain the finished product of monoammonium glycyrrhizinate.

Embodiment 3

[0011] Example 3: Dissolve 1Kg of glycyrrhizic acid powder in a mixed solvent of 5Kg by weight of ethanol and acetone with a concentration of 90% and reflux 4 times, each time for 1 hour to obtain an extract. The mixture of ethanol and acetone is 1:1, and filter through 180um Cloth, combined filtrates, added ammonia gas to the obtained extract until the pH value was between 5 and 6 and stirred for 30min, then left to stand for 1h, passed through a 149um filter cloth, and the resulting precipitate was recrystallized with 4Kg of ethanol with a concentration of 75%. Once dried until the water content is below 8%, the monoammonium glycyrrhizinate is obtained.

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PUM

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Abstract

The invention discloses a method for preparing mono-ammonium glycyrrhizinate, consisting essentially of the following processing steps of: dissolving glycyrrhizic acid powder into organic solvent solution for refluxing extraction; adding ammonia or ammonia water; and obtaining the mono-ammonium glycyrrhizinate after filtering and drying. The preparation method takes the glycyrrhizic acid powder as raw material to directly prepare mono-ammonium glycyrrhizinate, the operation is simple and convenient, the time is saved, the cost is reduced, and the product content is high, thus avoiding the drawbacks in the existing preparation process of the mono-ammonium glycyrrhizinate such as long steps, high cost, use of a large amount of organic solvent, not being beneficial to environmental protection, low product content, and the like.

Description

technical field [0001] The invention relates to a preparation method of monoammonium glycyrrhizinate. technical background [0002] Glycyrrhizinate monoammonium salt is the third generation substitute of the active ingredient of traditional Chinese medicine licorice, and it has strong anti-inflammatory, liver cell membrane protection and liver function improvement effects. At present, the synthesis method of glycyrrhizinate monoammonium salt is generally prepared from licorice Glycyrrhizic acid powder, and first by synthesizing triammonium glycyrrhizinate, then adding acetic acid to prepare monoammonium glycyrrhizinate, the process is many, the process is complicated, the production cost is high, and needs to use a large amount of solvent, the solvent used is not conducive to environmental protection, and the product content obtained lower. Invention content: [0003] In order to overcome the deficiencies in the prior art, the purpose of the present invention is to provid...

Claims

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Application Information

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IPC IPC(8): C07J63/00
Inventor 陈振鸿
Owner XINJIANG FUWO PHARMA
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