Glycyrrhetinic acid preparation method

A technology of glycyrrhetinic acid and licorice extract, which is applied in the field of biomedicine, can solve the problems of long hydrolysis time, long conversion time, and low efficiency, and achieve the effects of reducing solvent consumption, shortening reaction time, and expanding the range of raw materials

Inactive Publication Date: 2015-04-08
普凡生生物科技(北京)股份有限公司
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Problems solved by technology

[0004] At present, there are mainly chemical methods and microbial methods for the conversion of glycyrrhetinic acid at home and abroad. The conversion time of microbial methods is long and the efficiency is low, which is not conducive to industrial production.
Chemical methods usually use high-purity glycyrrhizinate or glycyrrhizic acid as raw materials, hydrolysis with sulfuric acid, filtration, long hydrolysis time, low conversion rate, difficult slag removal, and high-purity products cannot be obtained
[0005] In the invention patent with the application number CN101817867B and the invention title "A Preparation Method of Glycyrrhetinic Acid", Gao Ying et al. used chemical methods to convert glycyrrhizic acid or glycyrrhizinate into acetylglycyrrhetinic acid, and then further deacetylated it to obtain licorice Secondary acid, this method has a high conversion rate, but the conversion time is longer, and deacetylation takes 3-6h

Method used

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  • Glycyrrhetinic acid preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Embodiment 1, the preparation of glycyrrhetinic acid

[0039] Such as figure 1 As shown, take licorice cream (9% glycyrrhizic acid content, HPLC method) 400g, add 50% (v / v) acetic acid aqueous solution 2400mL, set ultrasonic power to 300W to extract 60min, filter to remove filter residue, then add catalyst concentrated sulfuric acid (98.3wt %) 12mL, set the ultrasonic power to 300W, and react for 60min. The obtained solid acetylglycyrrhetinic acid was filtered, washed with 200 mL of water, and dried at a material temperature of 60°C. 25.12 g of acetylglycyrrhetinic acid was obtained with a purity of 90.5%.

[0040] Weigh 20.3g of the above-mentioned acetylglycyrrhetinic acid; add NaOH solution (20.3mL) with a concentration of 5mol / L; put it into an ultrasonic reactor for reaction for 60min, and the ultrasonic power is 100W; Cake to remove salts; filter cake drying to obtain crude product glycyrrhetinic acid 17.8g; crude product glycyrrhetinic acid was added 20 times ...

Embodiment 2

[0041] Embodiment 2, the preparation of glycyrrhetinic acid

[0042] Such as figure 1 As shown, take glycyrrhizic acid powder (22% glycyrrhizic acid content, HPLC) 200g, add 70% (v / v) acetic acid aqueous solution 1000mL, set the ultrasonic power to 500W to extract 45min, filter to remove filter residue, then add catalyst concentrated sulfuric acid (98.3wt %) 6mL, set the ultrasonic power to 500W, and react for 45min. The obtained solid acetylglycyrrhetinic acid was filtered, washed with 300 mL of water, and dried at a material temperature of 60°C. 38.46 g of acetylglycyrrhetinic acid was obtained with a purity of 92.3% (HPLC).

[0043]Weigh 20.5g of the above-mentioned acetylglycyrrhetinic acid; add KOH solution (41mL) with a concentration of 4mol / L; put it into an ultrasonic reactor for 90min, and the ultrasonic power is 300W; after the reaction is completed, lower it to 25°C, filter, and wash the filter cake with water , to remove salts; the filter cake was dried to obtai...

Embodiment 3

[0044] Embodiment 3, the preparation of glycyrrhetinic acid

[0045] Such as figure 1 As shown, get 200 g of monoammonium glycyrrhizic acid (70% HPLC content of glycyrrhizic acid), add 800 mL of 90% (v / v) acetic acid aqueous solution, set the ultrasonic power to 700 W and extract for 30 min, remove the filter residue by filtration, then add catalyst concentrated sulfuric acid (98.3 wt%) 12mL, set the ultrasonic power to 700W, and react for 30min. Filter the obtained solid acetylglycyrrhetinic acid, rinse with 400 mL of water, and dry at a material temperature of 60°C. 60.38 g of acetylglycyrrhetinic acid was obtained with a purity of 95.5% (HPLC).

[0046] Weigh 20.4g of the above-mentioned acetylglycyrrhetinic acid; add NaOH solution (81.6mL) with a concentration of 2mol / L; put it into an ultrasonic reactor for reaction for 60min, and the ultrasonic power is 500W; Cake to remove salts; the filter cake was dried to obtain crude product glycyrrhetinic acid 18.1g; crude produ...

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Abstract

The invention discloses a glycyrrhetinic acid preparation method which comprises the following steps: (1) filter liquor is obtained by ultrasonic extraction of licorice extract, the licorice extract comprises 9%-70% by mass of glycyrrhizic acid; (2) under ultrasonic conditions, a catalyst is added to the filter liquor for the acetylation to obtain acetyl glycyrrhetinic acid; the catalyst is any one of sulfuric acid, hydrochloric acid and phosphoric acid; and (3) in the presence of ultrasonic and alkaline conditions, the glycyrrhetinic acid is obtained by deacetylation of the acetyl glycyrrhetinic acid. According to the method, by ultrasonic extraction and ultrasonic reaction technology, the reaction time is significantly shortened, the solvent consumption is reduced, environmental pollution is little, side reaction is less, the conversion rate is obviously improved, the liquorice extract is used as a raw material, the raw material range is expanded, the problems of high raw material cost, long reaction time, serious environmental pollution and the like are solved, production cost is low, product purity is high, and the method is suitable for mass production.

Description

technical field [0001] The invention relates to a preparation method of glycyrrhetinic acid, in particular to a method for ultrasonically assisted preparation of glycyrrhetinic acid, which belongs to the field of biomedicine. Background technique [0002] Licorice is a traditional Chinese medicinal material with a long history of application and is well-known at home and abroad. As early as the Warring States period, there were records of using licorice to treat diseases, more than 2,500 years ago. "Shen Nong's Materia Medica" in the Eastern Han Dynasty called licorice "beautiful grass" and "sweet sweetness", and listed it as top grade. Traditional Chinese medicine believes that: licorice is sweet and flat, and it is a good medicine for invigorating the spleen and Qi, relieving coughs and diseases, relieving spasms and pains, harmonizing various medicines, and detoxifying. The US FDA lists licorice extract as a safe and non-toxic substance. [0003] Glycyrrhizic acid, the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
CPCC07J63/008
Inventor 高彦祥杨新涛王海林
Owner 普凡生生物科技(北京)股份有限公司
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