Method for preparing glycyrrhetinic acid

A technology of glycyrrhetic acid and glycyrrhizic acid powder is applied in the directions of steroids, organic chemistry, etc., can solve the problems of complicated preparation conditions and process technology, high cost, difficult to realize industrialization, etc., achieves low production cost, reduced equipment requirements, The effect of easy control of the process

Active Publication Date: 2010-09-01
甘肃泛植制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although pure glycyrrhetinic acid can be obtained by enzymatic hydrolysis, the preparation conditions and process technology are complicated, the cost is high, and it is not easy to realize industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take 140g of glycyrrhizic acid powder (the content of glycyrrhizic acid is about 25% HPLC), add 1120ml of 95% edible ethanol, extract at 40°C for 3 hours, filter to remove insoluble impurities, distill the filtrate to recover ethanol to obtain the extract, and dry the extract on a water bath at 100°C , to obtain 118g of dry extract with a moisture content of not more than 20%; after crushing the dry extract, take 100g, add 300ml of 70% glacial acetic acid, add 7ml of concentrated sulfuric acid, hydrolyze and acetylate under normal pressure, and heat up to 98-103°C, React for 2 hours, after hydrolysis and acetylation are completed, cool to room temperature, filter the precipitated solid, wash the filter cake with 250ml 65% acetic acid, wash with 200ml ethanol, and finally wash with 300ml water, dry at 100°C to obtain acetyl Glycyrrhetinic acid crude product 20.21g, purity 88.2% (HPLC).

[0016] Take 20g of acetylglycyrrhetinic acid, add 300ml of water, add 5g of sodium h...

Embodiment 2

[0018] Take 140g of glycyrrhizic acid powder (the content of glycyrrhizic acid is about 25% HPLC), add 980ml of methanol, extract at room temperature for 1.5 hours, filter to remove insoluble impurities, and distill the filtrate to recover methanol to obtain an extract, which is dried on a water bath at 80°C to obtain 120g dry extract with a water content not greater than 20%; crush the dry extract and take 100g, add 500ml of 60% glacial acetic acid, add 24ml of concentrated hydrochloric acid, heat up to 85-90°C for hydrolysis and acetylation, and react for 4 hours until hydrolysis And after the acetylation is completed, cool to room temperature, filter and separate out the solid matter, wash the filter cake with 250ml of 65% acetic acid, wash with 200ml of methanol, and finally wash with 300ml of water, and dry at 80°C to obtain 20.38g of the crude product of acetylglycyrrhetinic acid. Purity 87.0% (HPLC).

[0019] Take 20g of acetylglycyrrhetinic acid, add 200ml of methanol,...

Embodiment 3

[0021] Take 140g of glycyrrhizic acid powder (about 25% HPLC of glycyrrhizic acid), add 4200ml of acetone, extract at 50°C for 5 hours, filter to remove insoluble impurities, distill the filtrate to recover ethanol to obtain the extract, and dry the extract at 90°C to obtain 110g dry extract with a water content not greater than 20%; crush the dry extract and take 100g, add 200ml of 85% glacial acetic acid, add 4.2ml of phosphoric acid, heat up to 95-98°C, hydrolyze and acetylate under normal pressure, and react 3 After hydrolysis and acetylation are completed, cool to room temperature, filter and separate out solid matter, wash the filter cake with 250ml 65% acetic acid, then wash with 200ml acetone, and finally wash with 300ml water, dry at 90°C to obtain acetylglycyrrhetinic acid Crude product 20.3g, purity 91.2% (HPLC).

[0022] Take 20g of acetylglycyrrhetinic acid, add 360ml of water, add 5g of sodium hydroxide to adjust the pH to 12, hydrolyze under normal pressure for ...

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Abstract

The invention provides a method for preparing glycyrrhetinic acid, which comprises the followings steps of: dissolving glycyrrihizic acid powder with an organic solvent, and extracting and purifying to obtain an extract; in acetic acid, performing catalytic hydrolysis of mineral acid and acetylation to obtain acetyl glycyrrhetinic acid; adding water or alcohol into the acetyl glycyrrhetinic acid,and hydrolyzing under the catalysis of alkali to obtain crude glycyrrhetinic acid; dissolving with an organic solvent, adding active carbon for refluxing and decoloring, and crystallizing to obtain the glycyrrhetinic acid of which the purity is over 97 percent (by a neutralization process); and further crystallizing for multiple times with the organic solvent to obtain the glycyrrhetinic acid with the purity over 98 percent (HPLC). In the method, the glycyrrihizic acid powder is used as a raw material, so the raw material range is widened; the production is carried out under normal pressure, pressure containers are not needed, and the requirement on equipment is low; and the process is easily controlled, the process technology is simplified, and the production cost is low.

Description

technical field [0001] The invention belongs to the technical field of medical raw materials, and in particular relates to a preparation method of glycyrrhetinic acid, a raw material medicine. Background technique [0002] Glycyrrhetinic acid is one of the deep processing products of licorice extract. Licorice is a commonly used traditional Chinese medicine, widely used in medicine, tobacco, food and other fields. Its main active ingredient, glycyrrhizic acid, has corticotropic hormone-like effects and can be used for detoxification, anti-inflammation, antitussive, anti-tumor, etc. The aglycone of glycyrrhizic acid is glycyrrhetinic acid. In the human body, glycyrrhizic acid is hydrolyzed by gastric acid or decomposed by β-glucuronidase in the liver to form glycyrrhetinic acid. The pharmacological effect of glycyrrhizic acid is essentially the effect of glycyrrhetinic acid. Pharmacological studies in recent years have found that the drugs of glycyrrhizic acid and glycyrrh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
Inventor 高颖李绍白李冲王兆瑞
Owner 甘肃泛植制药有限公司
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