Method for rapidly extracting and purifying glycyrrhizic acid and salts thereof

A technology of glycyrrhizinate and extraction method, which is applied in the direction of chemical instruments and methods, organic chemistry, steroidal compounds, etc., can solve the problems of low extraction efficiency, 2-6 hours, and large amount of extracting solution, so as to improve product quality , shorten the extraction time, reduce the effect of waste liquid volume

Inactive Publication Date: 2014-11-19
EAST CHINA UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The extraction efficiency of methods such as cold soaking and seepage is very low, and the extraction time often takes more than 24 hours, and the amount of extracting liquid is large, and the energy consumed for concentrating the extracting liquid is relatively large
Methods such as hot soaking and heat reflux shorten the extraction time to 2-5 hours by heating the extract (generally 40-80°C), but the content of protein, starch, polysaccharides, etc. in the obtained extract increases, thus affecting the purity and color of the product
The microwave-assisted extraction method and the ultrasonic-assisted extraction method further shorten the extraction time to 20-60 minutes, and the extraction temperature is also reduced to 30-50°C through microwave, ultrasonic and other enhanced mass transfer processes. Disadvantages such as large energy consumption of liquid
The supercritical extraction method uses supercritical carbon dioxide as the extraction solvent, and modifiers such as methanol and ethanol are often added to increase its polarity. Due to the low polarity of the solvent, the extraction effect on glycyrrhizic acid is limited, and the extraction time usually takes 2-6 hours , and need to use high-pressure equipment (the pressure is generally greater than 100 atmospheres), and the investment cost is relatively high

Method used

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  • Method for rapidly extracting and purifying glycyrrhizic acid and salts thereof
  • Method for rapidly extracting and purifying glycyrrhizic acid and salts thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0127] Preparation of Glycyrrhizic Acid Powder by Flash Water Extraction

[0128] Glycyrrhiza rhizomes are crushed and passed through a 40-mesh standard sieve to obtain licorice powder. Take 20 g of licorice powder, disperse it with 400 mL of deionized water, place it in a flash extractor, and extract it at room temperature at 10,000 rpm for 5 minutes to obtain an extract. Filtrate was obtained by filtration, and the pH was adjusted to 2.0-2.5 with concentrated sulfuric acid; glycyrrhizic acid was precipitated, centrifuged, and the obtained precipitate was washed with a small amount of water, then centrifuged again, and the precipitate was vacuum-dried at 35°C to obtain glycyrrhizic acid powder. The purity of glycyrrhizic acid was 25.3% by HPLC analysis.

[0129] After the supernatant obtained from the above centrifugation process was combined, calcium hydroxide powder was added to adjust the pH to 7.0-7.5 to form calcium sulfate precipitate, which was settled for half an hou...

Embodiment 2

[0136] Preparation of Monoammonium Glycyrrhizinate Coarse Powder by Flash Alcohol Extraction

[0137] The glycyrrhizic acid powder prepared by the flash extraction method was crushed and passed through a 40-mesh standard sieve. Take 5g of glycyrrhizic acid powder, disperse it with 100mL of 95wt% ethanol, place it in a flash extractor, and extract it at room temperature at 10,000 rpm for 5 minutes to obtain an extract. The filtrate was obtained by filtration, and the pH was adjusted to 8.0-8.5 with 22-25% concentrated ammonia water; triammonium glycyrrhizinate precipitated, filtered, and about 3 g of the obtained filter cake was dissolved by heating with 6 mL of glacial acetic acid at 60°C. After cooling, monoammonium glycyrrhizinate precipitated out. Filtrate to obtain crude wet crystals of monoammonium glycyrrhizinate, wash with 3 mL of glacial acetic acid and 3 mL of absolute ethanol in turn, and then dry in a vacuum desiccator at 35°C for more than 8 hours. The purity of ...

Embodiment 3

[0144] Preparation of Monopotassium Glycyrrhizinate Coarse Powder by Flash Alcohol Extraction

[0145] The glycyrrhizic acid powder prepared by the flash extraction method was crushed and passed through a 40-mesh standard sieve. Take 5g of glycyrrhizic acid powder, disperse it with 100mL of 95wt% ethanol, place it in a flash extractor, and extract it at room temperature at 10,000 rpm for 5 minutes to obtain an extract.

[0146] The filtrate was obtained by filtration, and the pH was adjusted to 8.0-8.5 with 20 wt% potassium hydroxide ethanol solution; tripotassium glycyrrhizinate precipitated out, filtered, and about 3 g of the obtained filter cake was dissolved by heating at 60° C. with 6 mL of glacial acetic acid. After cooling, monopotassium glycyrrhizinate precipitated out.

[0147] Filtrate to obtain wet crystals of crude monopotassium glycyrrhizinate, wash with 3 mL of glacial acetic acid and 3 mL of absolute ethanol in turn, and then dry in a vacuum desiccator at 35°C ...

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Abstract

The invention discloses a method for rapidly extracting and purifying glycyrrhizic acid and salts thereof. The method comprises the steps of: by taking licorice rhizomes as a raw material, preparing glycyrrhizic acid by using a flash extraction technology; by taking glycyrrhizic acid powder as a raw material, preparing glycyrrhetates by using the flash extraction technology. According to the method disclosed by the invention, an effect of rapid extraction at room temperature is achieved; compared with existing processes, the cyclic utilization of solvents can be realized, thereby significantly reducing the amount of waste liquid, reducing the energy consumption, shortening the extraction time, and improving the quality of products.

Description

technical field [0001] The invention relates to the field of separation and purification of active components of Chinese herbal medicines, in particular to a method for rapidly extracting and purifying glycyrrhizic acid and its salts. Background technique [0002] Licorice is one of the commonly used traditional Chinese medicine varieties in my country. It is rich in active ingredients such as triterpenoid saponins, flavonoids, and polysaccharides. The active ingredient with the highest content in licorice is glycyrrhizic acid. Glycyrrhizic acid is a triterpenoid saponin compound, and it is also the active component of licorice that has been studied thoroughly and widely used. In particular, high-purity glycyrrhizic acid and its salts can be prepared into popular drugs such as glycyrrhetinic acid, magnesium isoglycyrrhizinate, and diammonium glycyrrhizinate through chemical reactions (CN200410083052.6), and the market demand is huge. [0003] There are many studies on the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00C07H15/256C07H1/08C07H1/00
Inventor 刘昌胜余金鹏徐向君袁媛喻玲杰梁生辉
Owner EAST CHINA UNIV OF SCI & TECH
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