Preparation method of diammonium glycyrrhizinate salt capable of accurately controlling ammonium radical content

A technology of diammonium glycyrrhizinate and diammonium glycyrrhizinate, which is applied to the preparation of sugar derivatives, chemical instruments and methods, and color/spectral property measurement, can solve problems such as differences in configuration and composition, and achieve improved yields and reduced Effect of the crystallization step

Active Publication Date: 2010-12-15
BEIJING UNION PHARMA FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Shockingly, we found that the marketed diammonium glycyrrhizinate products tested were actually basically monoammonium salts; even more disturbing, we found that the marketed diammonium glycyrrhizinate products tested were actually all 18α , 18β-configuration mixture (18α-configuration accounts for about 70% to 80%, 18β-configuration accounts for about 30% to 20%), but there are large differences in the configuration composition of products from different manufacturers

Method used

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  • Preparation method of diammonium glycyrrhizinate salt capable of accurately controlling ammonium radical content
  • Preparation method of diammonium glycyrrhizinate salt capable of accurately controlling ammonium radical content
  • Preparation method of diammonium glycyrrhizinate salt capable of accurately controlling ammonium radical content

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Embodiment 1: Preparation of diammonium glycyrrhizinate by adopting known and satisfactory monoammonium glycyrrhizinate mainly in 18α ​​configuration

[0061] (1) Take 50 g of monoammonium glycyrrhizinate, add 100 mL of water, heat and stir to dissolve, add about 11 mL of 6.8% ammonia water to adjust the pH value to 4.6.

[0062] (2) The above liquid medicine is added to a stainless steel plate, vacuum freeze-dried, vacuumized, the temperature of the product is controlled below -10°C for primary sublimation, the temperature is raised after the water is basically removed, and the temperature of the product is controlled below 40°C for secondary drying. The final product was obtained as off-white loose solid.

[0063] (3) The product yield is basically 100%.

[0064] (4) Test results of configuration and ammonium root content: The measured 18α configuration accounts for 76.4%, and the ammonium root content is 77.3%.

Embodiment 2

[0065] Embodiment 2: Preparation of diammonium glycyrrhizinate by adopting the monoammonium glycyrrhizinate mainly in 18α ​​configuration known to meet the requirements

[0066] (1) Take 50 g of monoammonium glycyrrhizinate, add 100 mL of water, heat and stir to dissolve, add about 13 mL of 13.6% ammonia water to adjust the pH value to 6.0.

[0067] (2) The above liquid medicine is added to a stainless steel plate, vacuum freeze-dried, vacuumized, the temperature of the product is controlled below -10°C for primary sublimation, the temperature is raised after the water is basically removed, and the temperature of the product is controlled below 40°C for secondary drying. The final product was obtained as off-white loose solid.

[0068] (3) The product yield is basically 100%.

[0069] (4) Test results of configuration and ammonium root content: the measured 18α configuration accounts for 75.2%, and the ammonium root content is 106.7%.

Embodiment 3

[0070] Embodiment 3: Preparation of diammonium glycyrrhizinate by adopting known and satisfactory monoammonium glycyrrhizinate mainly in 18α ​​configuration

[0071] (1) Take 1000 g of monoammonium glycyrrhizinate, add 2000 mL of water, heat and stir to dissolve, add about 260 mL of 6.8% ammonia water to adjust the pH value to 4.8.

[0072] (2) The above liquid medicine is added to a stainless steel plate, vacuum freeze-dried, vacuumized, the temperature of the product is controlled below -10°C for primary sublimation, the temperature is raised after the water is basically removed, and the temperature of the product is controlled below 40°C for secondary drying. The final product was obtained as off-white loose solid.

[0073] (3) The product yield is basically 100%.

[0074] (4) Test results of configuration and ammonium root content: The measured 18α configuration accounts for 76.3%, and the ammonium root content is 88.7%.

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Abstract

The invention relates to a preparation method of a diammonium glycyrrhizinate salt capable of accurately controlling ammonium radical content, which is characterized by comprising the following steps of: using a mono-ammonium glycyrrhizinate salt as an initiative raw material; dissolving by adding a protic solvent; regulating a pH value as 4.5-9.0 by adding ammonia; drying by using a suitable method; and monitoring the ammonium radical content by adopting indophenol blue colorimetry to consequently prepare the diammonium glycyrrhizinate salt with correct ammonium radical content. A preparation technology and a monitoring method of the invention solve the problem of wrong ammonium radical content of the diammonium glycyrrhizinate salt prepared by the prior art in a breakthrough mode, reduce crystallizing steps at the same time, greatly increase the diammonium salt yield and are suitable for industrialized production. The prepared diammonium glycyrrhizinate salt also has definite18alpha and 18beta configurational compositions.

Description

technical field [0001] The invention relates to a preparation method of diammonium glycyrrhizinate salt capable of accurately controlling the ammonium root content, and the application of an indophenol blue colorimetric method capable of accurately monitoring the ammonium root content in the preparation process. Background technique [0002] Glycyrrhizic acid is the main active substance in the traditional Chinese medicine licorice. The molecular structure of glycyrrhizic acid core is as follows: [0003] [0004] The molecular structure has the following two characteristics: [0005] First, there are three carboxyl groups in the structure, which may form monoammonium salt, diammonium salt or triammonium salt. [0006] Second, there is an isomer center at 18H (marked "*" in the structure diagram), which can form isomers of 18α and 18β configurations. The molecular structures of these two isomers are as follows: [0007] [0008] 18α-Glycyrrhizic acid 18β-Glycyrrhizi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00C07H15/256C07H1/00G01N21/31
Inventor 吕昭云吕亚光潘显道张猛陈洋尹明福李强张世勇姚瑞赵立敏
Owner BEIJING UNION PHARMA FACTORY
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