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Method for preparing glycyrrhizic acid derivatives by carrying out subcritical hydrolysis reaction

A hydrolysis reaction, glycyrrhizic acid technology, applied in the preparation of sugar derivatives, sugar derivatives, sugar derivatives and other directions, can solve the problems of complex preparation process, long cycle and high cost, and achieve high product yield, low cost, and high production efficiency. Efficient effect

Active Publication Date: 2015-03-04
CHINA AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the present invention is to provide a method for preparing glycyrrhizic acid derivatives by subcritical hydrolysis for the problems of complex preparation process, high cost, long period, low yield and serious pollution in the prior art

Method used

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  • Method for preparing glycyrrhizic acid derivatives by carrying out subcritical hydrolysis reaction
  • Method for preparing glycyrrhizic acid derivatives by carrying out subcritical hydrolysis reaction
  • Method for preparing glycyrrhizic acid derivatives by carrying out subcritical hydrolysis reaction

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Embodiment 1

[0028] according to figure 1 The process flow diagram of the preparation of glycyrrhizic acid derivatives by the subcritical hydrolysis reaction shown, prepares monoglucuronic acid glycyrrhetinic acid and glycyrrhetinic acid through subcritical hydrolysis reaction from glycyrrhizic acid, comprising the following steps:

[0029] (1) Raw material dissolution: Dissolve glycyrrhizic acid in 30% ethanol-water solution at 65°C, then add acetic acid to adjust pH=3 to obtain a glycyrrhizic acid solution with a concentration of 1.8%;

[0030] (2) Subcritical hydrolysis reaction: pump the glycyrrhizic acid solution into the subcritical reaction kettle through a high-pressure infusion pump, and carry out stirring reaction under high temperature and high pressure. The reaction temperature is 120°C, the pressure is 5MPa, the time is 50min, and the stirring speed is 100rpm , after the reaction finishes, collect the reaction solution;

[0031] (3) Centrifugal treatment: the above reaction s...

Embodiment 2

[0039] This embodiment discloses a method for preparing glycyrrhetinic acid monoglucuronate and glycyrrhetinic acid from glycyrrhizic acid through subcritical hydrolysis reaction, comprising the following steps:

[0040] (1) Raw material dissolution: Dissolve glycyrrhizic acid in 70% ethanol-water solution at 65°C, then add acetic acid to adjust pH=2 to obtain a glycyrrhizic acid solution with a concentration of 1.8%;

[0041] (2) Subcritical hydrolysis reaction: pump the glycyrrhizic acid solution into the subcritical reaction kettle through a high-pressure infusion pump, and carry out stirring reaction under high temperature and high pressure. The reaction temperature is 160°C, the pressure is 9MPa, the time is 20min, and the stirring speed is 200rpm , after the reaction finishes, collect the reaction solution;

[0042] (3) Centrifugal treatment: the above reaction solution was centrifuged to obtain a clarified liquid, the centrifugal speed was 4200rpm, and the time was 10mi...

Embodiment 3

[0049] This embodiment discloses a method for preparing glycyrrhetinic acid monoglucuronate and glycyrrhetinic acid from glycyrrhizic acid through subcritical hydrolysis reaction, comprising the following steps:

[0050] (1) Raw material dissolution: Dissolve glycyrrhizic acid in 30% ethanol-water solution at 65°C, then add acetic acid to adjust pH=2 to obtain a glycyrrhizic acid solution with a concentration of 3.6%;

[0051] (2) Subcritical hydrolysis reaction: pump the glycyrrhizic acid solution into the subcritical reaction kettle through a high-pressure infusion pump, and carry out stirring reaction under high temperature and high pressure. The reaction temperature is 140°C, the pressure is 7MPa, the time is 70min, and the stirring speed is 150rpm , after the reaction finishes, collect the reaction solution;

[0052] (3) Centrifugal treatment: the above reaction solution was centrifuged to obtain a clarified liquid, the centrifugal speed was 4200rpm, and the time was 10mi...

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Abstract

The invention discloses a method for preparing glycyrrhizic acid derivatives by carrying out a subcritical hydrolysis reaction and belongs to the technical field of biochemical engineering. Glycyrrhizic acid or liquorice extract is taken as a raw material, and glycyrrhetinic acid and glycyrrhetinic acid 3-O-glucuronide are prepared by carrying out the subcritical hydrolysis reaction. The method for preparing the glycyrrhizic acid derivatives by carrying out the subcritical hydrolysis reaction comprises the following steps: firstly dissolving raw materials to obtain a glycyrrhizic acid solution, then carrying out the subcritical hydrolysis reaction to prepare a reaction liquid, and centrifuging, separating, concentrating or redissolving and drying the reaction liquid, so that glycyrrhetinic acid 3-O-glucuronide and glycyrrhetinic acid are obtained. The method for preparing the glycyrrhizic acid derivatives by carrying out the subcritical hydrolysis reaction has the advantages that a preparation technology is scientific and reasonable, operation is simple and feasible, cost is low, continuous production can be realized, and the glycyrrhizic acid derivative products are easy to popularize and have a higher additional value; the amount of acid added in a preparation process is little, no destructive effect is produced to a structure of glycyrrhizic acid, product yield is high, and no pollution to the environment is produced; and the glycyrrhizic acid derivative products can be taken as a food additive and a medicine precursor substance and raw materials are provided for the food and pharmaceutical industries.

Description

technical field [0001] The invention belongs to the technical field of biochemical industry, and in particular relates to a method for preparing glycyrrhizic acid derivatives by subcritical hydrolysis. Background technique [0002] Glycyrrhizauralensis, also known as sweet grass root, red licorice, old country, sweet grass, sweet root, etc., is one of the traditional Chinese herbal medicines commonly used in my country. Licorice is flat and sweet in nature, has the functions of invigorating the spleen and replenishing qi, clearing heat and detoxification, eliminating phlegm and relieving cough, relieving spasms and relieving pain, and reconciling various medicines. It has extremely wide clinical application value. In my country, licorice is the most widely used herbal medicine among more than 2,000 kinds of herbal medicines. It is known as "nine herbs in ten directions, and no prescription without herbs". At the same time, licorice is one of the best natural sweeteners ever...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
CPCC07H1/00C07H15/256C07J63/008
Inventor 高彦祥樊蕊
Owner CHINA AGRI UNIV
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