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Method for preparing glycyrrhetinic acid

A technology of glycyrrhetinic acid and glycyrrhizic acid powder, which is applied in the field of medicine, can solve problems such as unsafe operation, incomplete hydrolysis, and long hydrolysis time, and achieve the effects of reducing pollution, low cost, and short hydrolysis time

Active Publication Date: 2012-10-24
GANSU YALAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Glycyrrhetinic acid is hydrolyzed by glycyrrhizic acid and acid. The hydrolysis requires a temperature of 100-110°C. If the temperature is too low, the hydrolysis time will be long and the hydrolysis will not be complete.
General solvents cannot reach this temperature under normal pressure, but pressurized hydrolysis requires high equipment and unsafe operation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1 A kind of preparation method of glycyrrhetinic acid comprises the following steps:

[0019] (1) Put 100kg of glycyrrhizic acid powder into a 2000L glass-lined reactor produced by Jiangsu Yangyang Chemical Equipment Co., Ltd., add 300L of water-saturated n-butanol and 3L of concentrated sulfuric acid in turn, and produce it with Wenzhou Jinbang Light Industry Equipment Factory after stirring and dissolving The DBYL800 type filter press is filtered to obtain filtrate A.

[0020] (2) The filtrate A was poured into a 2000L glass-lined reactor, heated to 105°C for hydrolysis, cooled to 20-40°C after 2 hours, and filtered with a DBYL800 filter press to obtain filtrate B.

[0021] (3) Filtrate B is recovered under reduced pressure with a 500kg / h glass-lined single-effect concentrator produced by Jiangsu Yangyang Chemical Equipment Co., Ltd. (the condition for reduced pressure recovery is 70°C, -0.06MPa) to 30L of n-butanol, add 30L of water , continue to concentr...

Embodiment 2

[0024] Embodiment 2 A kind of preparation method of glycyrrhetinic acid comprises the following steps:

[0025] (1) Put 100kg of glycyrrhizic acid powder into a 2000L glass-lined reactor, add 450L of water-saturated n-butanol and 5.5L of concentrated sulfuric acid successively, and filter with a DBYL800 filter press after stirring to dissolve to obtain filtrate A.

[0026] (2) The filtrate A was poured into a 2000L glass-lined reactor, heated to 100°C for hydrolysis, cooled to 20-40°C after 1 hour, and filtered with a DBYL800 filter press to obtain filtrate B.

[0027] (3) Filtrate B is recovered under reduced pressure with a 500kg / h glass-lined single-effect concentrator (the condition for recovery under reduced pressure is 70°C, -0.06MPa) to 45L of n-butanol, add 45L of water, and continue to concentrate until there is no n-butanol, Obtain the concentrated solution; the concentrated solution is suction-filtered with an 800-type glass-lined suction filter, filtered to obtain ...

Embodiment 3

[0030] Embodiment 3 A kind of preparation method of glycyrrhetinic acid comprises the following steps:

[0031] (1) Put 100kg of glycyrrhizic acid powder into a 2000L glass-lined reactor, add 600L of water-saturated n-butanol and 8L of concentrated sulfuric acid in sequence, and filter with a DBYL800 filter press to obtain filtrate A after stirring and dissolving.

[0032] (2) The filtrate A was poured into a 2000L glass-lined reactor, heated to 100°C for hydrolysis, cooled to 20-40°C after 0.5h, and filtered with a DBYL800 filter press to obtain filtrate B.

[0033] (3) Filtrate B is recovered under reduced pressure with a 500kg / h glass-lined single-effect concentrator (the condition for recovery under reduced pressure is 70°C, -0.06MPa) to 60L of n-butanol, add 60L of water, and continue to concentrate until there is no n-butanol, Obtain the concentrated solution; the concentrated solution is suction-filtered with an 800-type glass-lined suction filter, filtered to obtain a ...

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Abstract

The invention relates to a method for preparing glycyrrhetinic acid, and the method comprises the following steps of: (1) sequentially adding n-butyl alcohol and concentrated sulphuric acid into glycyrrhizic acid powder, and filtering after stirring and dissolving so as to obtain filtrate A; (2) heating and hydrolyzing the filtrate A and reducing temperature to be 20-40 DEG C, and filtering to obtain filtrate B; (3) carrying out reduced-pressure concentration on the filtrate B to recycle n-butyl alcohol until volume of the filtrate B is 10% of the original volume of n-butyl alcohol, adding water equivoluminal with recycled n-butyl alcohol, continuing concentrating until no n-butyl alcohol exists, and filtering to obtain precipitate; (4) washing the precipitate to be neutral, adding sodiumhydroxide solution, and filtering after the precipitate is dissolved so as to obtain filtrate C; and (5) adding hydrochloric acid into the filtrate C to regulate pH value to be 4-6, washing the precipitate obtained by regulating the pH value with water until the pH value is equal to 7, and then carrying out vacuum drying so as to obtain glycyrrhetinic acid. Glycyrrhetinic acid provided by the invention can be hydrolyzed at normal pressure and has high hydrolysis temperature, short hydrolysis time and high hydrolysis efficiency.

Description

technical field [0001] The invention relates to the field of medicine, in particular to a preparation method of glycyrrhetinic acid. Background technique [0002] Glycyrrhetinic acid has antibacterial, antitumor and adrenal cortex hormone-like effects, and can be made into anti-inflammatory and anti-allergic preparations for the treatment of rheumatoid arthritis, asthma, allergic and occupational dermatitis, inflammation and ulcers in ophthalmology, ear, nose and throat, etc. [0003] Glycyrrhetinic acid is a classic anti-inflammatory drug. Its application in cosmetics can regulate the immune function of the skin, enhance the skin's disease resistance, eliminate inflammation, prevent allergies, clean the skin, and at the same time relieve the effects of cosmetics and other external factors on the skin. toxic side effects. It can also effectively inhibit the activation of tyrosinase, prevent the production of melanin, and has whitening effect. [0004] Glycyrrhetinic acid i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J63/00
Inventor 董万有王卫国张继义张丹
Owner GANSU YALAN PHARMA
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