Process for extracting purified glycyrrhizic acid from licorice residue

A technology of glycyrrhizic acid and licorice residue, applied in the directions of organic chemistry, steroids, etc., can solve the problems of low extraction rate, long extraction time, and high product impurity content, and achieve the effect of high extraction rate and fast extraction speed.

Inactive Publication Date: 2003-10-22
NORTHEAST FORESTRY UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patented method involves creating an ultra sound wave that helps remove impurities from plants called caffeine or other compounds found naturally within them by breaking down into smaller molecules like sugars during processing. These small particles are then extracted through this process for further use such as making medicine.

Problems solved by technology

The technical problem addressed by this patented method described in the patents relates to traditional ways of obtaining pure ammoniumsulfonate from plants that contain these ingredients such as liquiritum officinale (L.) L., which can be expensive due to their complex composition.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Put 150 g of dried supercritical licorice residue into the reaction vessel of an ultrasonic extraction device, add 8 times the amount of 0.2% ammonia water, control the water temperature to 30° C., and perform ultrasonic extraction for 4 hours. The extraction rate of glycyrrhizic acid is 1.8032%. with 7NH 2 SO 4 Acidify the glycyrrhizic acid extract to a pH of 1.0, filter, and dry at room temperature to obtain crude glycyrrhizic acid. Take a certain amount of crude glycyrrhizic acid, add 7 times the amount of 80% ethanol to extract at 60 ° C for 2 hours, pass through the extract solution into ammonia gas to react to form triammonium glycyrrhizinate, filter, and react with glacial acetic acid to form monoammonium glycyrrhizinate. Crude salt. The crude product of monoammonium glycyrrhizinate salt is recrystallized, the solvent is 60% ethanol, the liquid-solid ratio is 2:1, the temperature is 80°C, heated for 20 minutes, filtered, placed to crystallize, the crystallized...

Embodiment 2

[0024] Put 150 g of dried supercritical licorice residue into the reaction vessel of an ultrasonic extraction device, add 9 times the amount of 0.25% ammonia water, control the water temperature at 40° C., and perform ultrasonic extraction for 5 hours. The extraction rate of glycyrrhizic acid is 2.0485%. with 7NH 2 SO 4 Acidify the glycyrrhizic acid extract to a pH of 2.0, filter, and dry at room temperature to obtain crude glycyrrhizic acid. Take a certain amount of crude glycyrrhizic acid, add 8 times the amount of 90% ethanol to extract at 65°C for 2 hours, pass through ammonia gas to react to form triammonium glycyrrhizinate, react with glacial acetic acid to form monoammonium glycyrrhizinate, filter, and use for precipitation The reaction of glacial acetic acid produces the crude product of monoammonium glycyrrhizinate. The crude product of monoammonium glycyrrhizinate salt was recrystallized, the solvent was 75% ethanol, the liquid-solid ratio was 3:1, the temperature ...

Embodiment 3

[0026] Put 150 g of dried supercritical licorice residue into the reaction vessel of an ultrasonic extraction device, add 10 times the amount of 0.3% ammonia water, control the water temperature at 50° C., and perform ultrasonic extraction for 6 hours. The extraction rate of glycyrrhizic acid is 2.1268%. with 7NH 2 SO 4 Acidify the glycyrrhizic acid extract to a pH of 3.0, filter, and dry at room temperature to obtain crude glycyrrhizic acid. Take a certain amount of crude glycyrrhizic acid, add 10 times the amount of 85% ethanol to extract at 70°C for 2 hours, pass through ammonia gas to react to form triammonium glycyrrhizinate, react with glacial acetic acid to form monoammonium glycyrrhizinate, filter, and use for precipitation The reaction of glacial acetic acid produces the crude product of monoammonium glycyrrhizinate. The crude product of monoammonium glycyrrhizinate salt is recrystallized, the solvent is 80% ethanol, the liquid-solid ratio is 4:1, the temperature is...

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Abstract

The method for extracting glycyrrhizic acid from licorice dregs and purifying it includes the following steps: supercritical licorice dregs drying, ultrasonic extracting, acidifying, soaking to make extraction, salifying, recrystallizing, drying to obtain ammonium glycyrrhizinate. Said invention has the characteristics of quick extraction speed, high extraction rate, small impurity content and easy purification, etc.

Description

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Claims

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Application Information

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Owner NORTHEAST FORESTRY UNIVERSITY
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