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Preparation method of glycyrrhizic acid

A technology of glycyrrhizic acid and licorice is applied in the preparation of sugar derivatives, chemical instruments and methods, steroids, etc., and can solve the problems of low glycyrrhizic acid content, unfavorable large-scale production operations, serious pollution, etc.

Inactive Publication Date: 2010-06-30
南京璇荣贸易有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the prior art, the extraction and separation method of glycyrrhizic acid mainly adopts organic solvent method, etc., but the content of glycyrrhizic acid obtained by these extraction processes is low, the pollution in the production process is serious, and it is unfavorable for large-scale production operations

Method used

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  • Preparation method of glycyrrhizic acid

Examples

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Comparison scheme
Effect test

Embodiment 1

[0018] Take 10Kg of fresh roots of licorice, add 3 times its weight in water and soak once for 12 hours each time, combine the liquid medicine, filter, adjust the filtrate with sulfuric acid, filter, take the filter residue, add methanol 3 times its weight in volume Reflux once, each time for 0.5 hours, combine the liquid medicine, add concentrated ammonia water to adjust pH7-8, recover methanol under reduced pressure until exhausted, add water to dissolve, adjust pH5-6 with sulfuric acid, absorb through AB-8 macroporous adsorption resin column, and water respectively and 5% ethanol for eluting, each collecting eluents of 1 times the volume of the column, merging, recovering the solvent under reduced pressure and drying to obtain glycyrrhizic acid coarse powder, adding acetic acid for recrystallization, washing and drying to obtain 72.8 g of glycyrrhizic acid. As detected by HPLC, the purity is 98.6%.

Embodiment 2

[0020] Take 10Kg of fresh roots of licorice, add 8 times its weight in water and soak for 3 times, each time for 36 hours, combine the medicinal solution, filter, the filtrate is adjusted with sulfuric acid, filter, take the filter residue, add methanol with 8 times its weight in volume Reflux 3 times, each time for 2 hours, combine the liquid medicine, add concentrated ammonia water to adjust pH7-8, recover methanol under reduced pressure until exhausted, add water to dissolve, adjust pH5-6 with sulfuric acid, adsorb through H-103 macroporous adsorption resin column, and water respectively and 40% ethanol for eluting, respectively collecting eluents of 5 times the volume of the column, merging, reclaiming the solvent under reduced pressure and drying to obtain glycyrrhizic acid coarse powder, adding acetic acid for recrystallization, washing and drying to obtain 94.3 g of glycyrrhizic acid. HPLC detection, the purity is 98.2%.

Embodiment 3

[0022] Take 10Kg of fresh roots of licorice, add 5 times its weight in water and soak twice, each time for 24 hours, combine the medicinal liquid, filter, adjust the filtrate with sulfuric acid, filter, take the filter residue, add methanol 5 times its weight in volume Reflux twice, each time for 1 hour, combine the liquid medicine, add concentrated ammonia water to adjust pH7-8, recover methanol under reduced pressure until exhausted, add water to dissolve, adjust pH5-6 with sulfuric acid, absorb through D101 macroporous adsorption resin column, water and 10 % ethanol for elution, collect eluents of 3 times the volume of the column, combine them, recover the solvent under reduced pressure and dry to obtain glycyrrhizic acid coarse powder, add acetic acid for recrystallization, wash and dry to obtain 96.8 g of glycyrrhizic acid, which is detected by HPLC , with a purity of 99.7%.

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Abstract

The invention relates to a preparation method of glycyrrhizic acid, which has the advantages of simple and convenient operation, little pollution and small equipment investment. The method comprises the following process steps: taking fresh liquorice roots to be added into water which accounts 3 to 8 times of the weight of the fresh liquorice roots for being soaked for 1 to 3 times (each time lasts 12 to 36 hours); merging and filtering medicine liquid; using sulphuric acid for regulating the filter liquor; filtering obtained materials; taking filter residue to be added into methanol which accounts for 3 to 8 times of the volume of filter residue for reversed flow for 1 to 3 times (each time lasts 0.5 to 2 hours); merging the medicine liquid; adding strong aqua ammonia to regulate the pH valve between 7 and 8; recovering all methanol through pressure reduction; adding water for dissolution; using sulphuric acid to regulate the pH value between 5 and 6; using macroporous absorbent resin posts for absorption; respectively using water and 5 to 40 percent ethanol for elution; respectively collecting eluent which accounts for 1 to 5 times of the volume of the macroporous absorbent resin posts; merging obtained materials; recovering solvents through pressure reduction; drying obtained materials to obtain glycyrrhizic acid coarse powder, and adding acetic acid for recrystallization. When the method of the invention is used for preparing the glycyrrhizic acid, the product purity is high, and the industrialized popularization can be easily realized.

Description

technical field [0001] The invention relates to a preparation method of glycyrrhizic acid, in particular to a method for extracting glycyrrhizic acid from plants. Background technique [0002] Glycyrrhizic acid (Glycyrrhizic acid), synonyms: glycyrrhizin, glycyrrhizin. Molecular formula: C 42 h 62 o 16 , molecular weight: 822.942, CAS accession number: 1405-86-3, the structural formula is as follows: [0003] [0004] Glycyrrhizic acid is a natural compound that has anti-inflammatory, cough-relieving and phlegm-reducing activities, and is widely found in many legume plants. [0005] The traditional Chinese medicine licorice is the dried root and rhizome of Glycyrrhiza uralensis Fisch., Glycyrrhiza inflata Bat. or Glycyrrhiza glabra L. of the leguminous plant Glycyrrhiza uralensis Fisch. It has the effects of invigorating the spleen and replenishing qi, clearing heat and detoxifying, eliminating phlegm and relieving cough, relieving spasms and relieving pain, reconcil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00C07H15/256C07H1/08
Inventor 张发成毛志英范淦彬
Owner 南京璇荣贸易有限公司
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