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Preparation method of monoammonium glycyrrhizinate

A technology of glycyrrhizic acid monoammonium salt and glycyrrhizic acid powder is applied in the preparation of sugar derivatives, chemical instruments and methods, steroid compounds, etc. , Easy to operate in large-scale production, high water solubility

Inactive Publication Date: 2020-12-08
张家港保税区麦福生物制品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the prior art, the method for preparing monoammonium glycyrrhizinate either adopts the traditional water extraction and alcohol precipitation method, which is inefficient; or adopts a new method that is not suitable for large-scale production operations. For example, a Chinese patent document CN106478761A discloses a method using Ultrafiltration crystallization method
In addition, when optimizing the preparation process of monoammonium glycyrrhizinate, those skilled in the art often only pay attention to conventional factors such as product purity and yield, and there is no report in the prior art that any process means affects the sweetness of the product

Method used

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  • Preparation method of monoammonium glycyrrhizinate
  • Preparation method of monoammonium glycyrrhizinate

Examples

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Effect test

Embodiment 1

[0059] Embodiment 1 Preparation of monoammonium glycyrrhizinate

[0060] (1) Extraction: Take glycyrrhizic acid powder (glycyrrhizic acid content is 25%), add 10L of ethanol aqueous solution (volume percentage concentration is 90%) for every 1Kg glycyrrhizic acid powder, stir and extract twice, filter, take Filtrate, marked as extract, for subsequent use;

[0061] (2) The first decolorization: Take the extract obtained in the previous step, add activated carbon, under the condition of heating (70-85 ℃), stir and decolorize, filter, take the filtrate, mark it as the primary decolorization solution, and set aside;

[0062] (3) Ammonia crystallization: Take the primary decolorization solution obtained in the previous step, raise the temperature to 60-65°C, slowly add ammonium acetate, keep it at 60-65°C for 25 minutes, lower the temperature to 40°C, slowly add formic acid, and then Raise the temperature to 60-65°C, keep the temperature at 60-65°C for 25 minutes, lower the temper...

Embodiment 2

[0068] The preparation of embodiment 2 monoammonium glycyrrhizinate

[0069] (1) Extraction: Take glycyrrhizic acid powder (30% glycyrrhizic acid content), add 15L of ethanol aqueous solution (volume percentage concentration: 94%) for every 1Kg glycyrrhizic acid powder, stir and extract once, filter, take Filtrate, marked as extract, for subsequent use;

[0070] (2) The first decolorization: Take the extract obtained in the previous step, add activated carbon, under the condition of heating (70-85 ℃), stir and decolorize, filter, take the filtrate, mark it as the primary decolorization solution, and set aside;

[0071] (3) Ammonia crystallization: Take the primary decolorization solution obtained in the previous step, raise the temperature to 60-65°C, slowly add ammonium acetate, keep it at 60-65°C for 45 minutes, lower the temperature to 25°C, slowly add formic acid, and then Raise the temperature to 60-65°C, keep the temperature at 60-65°C for 45 minutes, lower the temperat...

Embodiment 3

[0078] Embodiment 3 Preparation of monoammonium glycyrrhizinate

[0079] (1) Extraction: Take glycyrrhizic acid powder (38% glycyrrhizic acid content), add 12L of ethanol aqueous solution (volume percentage concentration: 92%) for every 1Kg glycyrrhizic acid powder, stir and extract twice, filter, take Filtrate, marked as extract, for subsequent use;

[0080] (2) The first decolorization: Take the extract obtained in the previous step, add activated carbon, under the condition of heating (70-85 ℃), stir and decolorize, filter, take the filtrate, mark it as the primary decolorization solution, and set aside;

[0081] (3) Ammonia crystallization: Take the primary decolorization solution obtained in the previous step, raise the temperature to 60-65°C, slowly add ammonium acetate, keep it warm at 60-65°C for 30 minutes, lower the temperature to 30°C, slowly add formic acid, and then Raise the temperature to 60-65°C, keep the temperature at 60-65°C for 30 minutes, lower the temper...

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Abstract

The invention relates to a preparation method of monoammonium glycyrrhizinate. The method comprises the following steps: (1) extraction; (2) primary decolorization; (3) ammonification crystallization:taking primary decolorizing liquid obtained in the previous step to heat to a temperature of 60 to 65 DEG C, slowly adding ammonium acetate, carrying out heat preservation for 25 to 45 minutes underthe condition of a temperature of 60 to 65 DEG C , cooling to a temperature of 25 to 40 DEG C, slowly adding formic acid, then heating to a temperature of 60 to 65 DEG C, carrying out heat preservation for 25 to 45 minutes under the condition of a temperature of 60 to 65 DEG C , cooling to a temperature of below 30 DEG C, stirring and crystallizing; (4) secondary decolorization; (5) crystallization and color washing; (6) drying; and (7) crushing, sieving and packaging. The method for preparing the monoammonium glycyrrhizinate is simple and convenient to operate, and the prepared product has high purity and sweetness.

Description

technical field [0001] The invention relates to a preparation method of glycyrrhizinate, in particular to a preparation method of glycyrrhizinate monoammonium salt. Background technique [0002] Glycyrrhizin is a class of natural sweeteners with various functional properties. Including glycyrrhizic acid and its salts, which are extracted from licorice roots and stems and obtained through purification. The products include glycyrrhizic acid, ammonium glycyrrhizinate, sodium glycyrrhizinate and potassium glycyrrhizinate. The structural formula of glycyrrhizic acid is triterpene saponin, and there are three carboxyl groups in the molecule, which can be in the form of mono-salt, di-salt, and tri-salt. Glycyrrhizinate is easily soluble in water and exhibits various functional properties in food processing. Because it is a natural compound extracted from plants, the U.S. Food and Drug Administration listed glycyrrhizin as the sweetest sweetener among "recognized safe substances...

Claims

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Application Information

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IPC IPC(8): C07H15/256C07H1/00C07H1/06C07J63/00
CPCC07H1/00C07H1/06C07H15/256C07J63/008
Inventor 葛方如陈文磊张振鹏
Owner 张家港保税区麦福生物制品有限公司
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