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Preparation method of sodium glycyrrhizinate and hydrates thereof

A technology of glycyrrhizic acid sodium salt and glycyrrhizic acid trisodium salt, which is applied in the direction of preparation of sugar derivatives, steroids, chemical instruments and methods, and can solve the problems of high cost, large investment in ultrafiltration, and small production volume.

Inactive Publication Date: 2015-06-24
李玉山
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the ultrafiltration method has a large investment and is rarely used now. The ion exchange method has a small processing capacity and needs to introduce exchangeable acidic or basic groups, which are rarely used at present. Preparative high-performance liquid chromatography requires Expensive instrument with small single preparation volume and few applications

Method used

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  • Preparation method of sodium glycyrrhizinate and hydrates thereof
  • Preparation method of sodium glycyrrhizinate and hydrates thereof
  • Preparation method of sodium glycyrrhizinate and hydrates thereof

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Embodiment Construction

[0017] Refining of glycyrrhizic acid: adding 100g of crude glycyrrhizic acid with a content of 75% to 300mL of n-butanol, extracting under reflux for 2.0h, pouring out the extract, and extracting the residue with 200mL of n-butanol under reflux for 1.5h, pouring out the extract, and refluxing the residue Extract with 100mL n-butanol under reflux for 1.0h. Combine 3 extracts, add 3-5% (W / V) 3-5% (W / W) activated clay and 3-5% (W / W) diatomaceous earth, incubate under reflux for 30min, filter, The filtrate was concentrated under reduced pressure to a specific gravity of 1.15-1.20, a small amount of ether was added, fully stirred, left to stand, crystallized, centrifuged, and the crystallized product was vacuum-dried at 60-70°C for 4-6 hours to obtain 71g of refined glycyrrhizic acid with a content of 99.5%.

[0018] Preparation of disodium glycyrrhizic acid: Dissolve 80g of glycyrrhizic acid with 320mL of n-butanol, add sodium carbonate to adjust the pH to 6-7, heat under reflux f...

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Abstract

The invention provides a preparation method of sodium glycyrrhizinate and hydrates thereof. The preparation method comprises the following steps: 1) preparing a crude product of glycyrrhizic acid; 2) preparing disodium glycyrrhizinate; 3) preparing a hydrate of disodium glycyrrhizinate; 4) preparing trisodium glycyrrhizinate; 5) preparing a hydrate of trisodium glycyrrhizinate. Glycyrrhizic acid and sodium hydroxide are adopted in traditional processes to generate trisodium glycyrrhizinate, two carboxyls with weaker acidity in glycyrrhizic acid are displaced through acidification of glacial acetic acid to obtain monosodium glycyrrhizinate, and then monosodium glycyrrhizinate is alkalized to obtain disodium glycyrrhizinate. 75% of crude product of glycyrrhizic acid is selected as the raw material and is refined to obtain a refined product of glycyrrhizic acid with content above 98%. Glycyrrhizic acid is used for generating different disodium glycyrrhizinate and hydrate thereof and trisodium glycyrrhizinate and hydrate thereof by controlling different pH values. The whole process is simple to operate, is mild in reaction conditions, is easy in control of quality, is high in conversion rate and is suitable for large-scale preparation.

Description

technical field [0001] The invention relates to a preparation method of glycyrrhizic acid sodium salt and hydrate thereof. Background technique [0002] Glyrrhizic acid, also known as glycyrrhizin and glycyrrhizin, is a triterpene saponin extracted from the dried roots and rhizomes of Glycyrrhiza uralensis fisch. It is a white or light yellow crystalline powder with a melting point of 220°C and a special sweet taste. . Molecular formula: C 42 h 62 o 16 , Molecular weight: 822.92. Glycyrrhizic acid in nature exists in two configurations of α-body and β-body, and the content of α-body is lower than 5% of β-body. The melting points of the two isomorphic crystals are 300-304°C and 287-293°C respectively, easily soluble in hot water and ethanol, and almost insoluble in ether. Its water-soluble salt has high sweetness, low heat energy, safety and non-toxicity, foaming and hemolysis, and is widely used in medicine, food, cosmetics and other industries. Glycyrrhizic acid has ...

Claims

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Application Information

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IPC IPC(8): C07J63/00C07H15/256C07H1/00
CPCC07H1/00C07H15/256C07J63/008
Inventor 李玉山
Owner 李玉山
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