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Method for continuous flow upstream abstraction purification of glycyrrhiza hypo-glycosides in glycyrrhizic acid biotransformation solution

A technology of biotransformation and glycyrrhetin, applied in the direction of steroids, organic chemistry, etc., can solve the problems of prolonged extraction reaching equilibrium, hindering the transfer of glycyrrhetin molecules, reducing the extraction efficiency of glycyrrhetin, etc., and prolonging the time to reach , easy continuous operation, fast and effective separation effect

Inactive Publication Date: 2010-12-15
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Glycyrrhizic acid biotransformation system is more complex and special than the countercurrent extraction system disclosed above
Glycyrrhizic acid and glycyrrhizin have relatively large surface activity, so when extracting glycyrrhizin from glycyrrhizic acid biotransformation solution by liquid-liquid extraction, severe emulsification is likely to occur, which seriously hinders the separation of glycyrrhizin molecules in the aqueous and organic phases. The transfer between them, and the emulsified layer is not easily damaged, which not only prolongs the time for the extraction to reach equilibrium, but also causes the entrainment of organic solvents in the emulsified layer, and at the same time causes the residual loss of glycyrrhetin in the emulsified layer, which eventually leads to the extraction of glycyrrhetin The efficiency is reduced, and these problems are expected to be improved by the countercurrent extraction method. At present, there are no publications or reports on the rapid purification of glycyrrhetin based on the continuous countercurrent extraction of the rotating disk column at home and abroad.

Method used

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  • Method for continuous flow upstream abstraction purification of glycyrrhiza hypo-glycosides in glycyrrhizic acid biotransformation solution
  • Method for continuous flow upstream abstraction purification of glycyrrhiza hypo-glycosides in glycyrrhizic acid biotransformation solution
  • Method for continuous flow upstream abstraction purification of glycyrrhiza hypo-glycosides in glycyrrhizic acid biotransformation solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] For the process of continuous countercurrent extraction and purification of glycyrrhetin, refer to the attached image 3 : the circulating water 1 of certain temperature is pumped into the turntable tower jacket 9 to keep the constant temperature; after adjusting the pH value of the glycyrrhizic acid biotransformation liquid with a certain glycyrrhetin content, it is added to the turntable tower with a certain flow rate from the heavy phase feeding port 2 At the same time, the extractant is fed into the tower body from the light phase feed port 3 at a flow rate corresponding to the heavy phase and is in countercurrent contact with the heavy phase. At the same time, the motor 6 drives the rotating shaft 8 and the turntable 10 to rotate to control a certain speed to promote the two-phase liquid. Fully mixed, Glycyrrhizin is separated from the aqueous phase solution and enters the organic extractant to form the upward aggregation of the extraction phase; after the extractio...

Embodiment 2

[0038] The implementation method and detection method of the present embodiment are the same as in Example 1, and the concrete parameters of implementation are as follows:

[0039] The extractant is ethyl acetate, the content of glycyrrhizin is 1.0g / L, the pH value is 4.5, the extraction temperature is 45°C, the flow rate of glycyrrhizic acid biotransformation solution is 15L / h, the flow ratio of extractant and glycyrrhizinic acid biotransformation solution is 1.5, the rotary speed of the turntable is 300rpm, and the solvent recovery method is vacuum distillation.

[0040] The yield of the product glycyrrhizin is 87.1%, and the purity is 95.2%.

Embodiment 3

[0042] The implementation method and detection method of the present embodiment are the same as in Example 1, and the concrete parameters of implementation are as follows:

[0043] The extractant is propyl acetate, the content of glycyrrhizin is 1.5g / L, the pH value is 4.8, the extraction temperature is 50°C, the flow rate of glycyrrhizic acid biotransformation solution is 20L / h, the flow ratio of extractant and glycyrrhizic acid biotransformation solution is 0.5, the feed liquid flow rate is 10L / h, the turntable speed is 200rpm, and the solvent recovery method is distillation.

[0044] The yield of the product glycyrrhizin is 89.2%, and the purity is 96.4%.

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Abstract

The invention relates to a method for continuously countercurrent extracting and purifying glycyrrhetinic glycoside in a glycyrrhizin biotransformation solution. The method is characterized in that: an extractant is added from the lower part of a turnplate tower; the glycyrrhizin biotransformation solution with a PH value of between 3.0 and 6.0 is added from the upper part of the turnplate tower,is subjected to continuous countercurrent liquid-liquid extraction at a temperature of between 30 and 60 DEG C and kept stand; an extraction phase is delaminated; and the extractant is separated and reclaimed for recycling, thereby obtaining a dried product of the glycyrrhetinic glycoside. The invention adopts a method of continuous countercurrent extraction and combines a method for adjusting the PH value of the glycyrrhizin biotransformation solution and controlling an extraction temperature, thereby realizing the rapid and effective separation of the glycyrrhetinic glycoside in a glycyrrhizin biotransformation system; and a purity of a separated glycyrrhetinic glycoside product reaches over 93.8 percent and a yield of the separated glycyrrhetinic glycoside product reaches over 92.5 percent.

Description

technical field [0001] The invention relates to an extraction and purification process of biotransformation products, in particular to a method for continuous countercurrent extraction and purification of glycyrrhizin in glycyrrhizic acid biotransformation solution. Background technique [0002] Glycyrrhetin, namely 18β-monoglucuronyl glycyrrhetinic acid (3-Monoglucuronyl-Glycyrrhetinic Acid, 3β-D-(monogluronyl) 18β-glycyrrhetic acid, referred to as GAMG), is a derivative of glycyrrhizic acid. Glycyrhetic acid (18β-GA) and a molecule of β-D-glucuronic acid (β-D-glucuronic acid, β-D-GluA). Under the catalysis of enzyme or acid, glycyrrhizic acid can be hydrolyzed to lose a glucuronic acid group to form glycyrrhetin. The hydrolysis of glycyrrhizic acid is shown in the attached figure 1 shown. [0003] Glycyrrhetin has inhibitory effect on hyaluronidase activity, also has inhibitory effect on contact dermatitis induced by m-trinitrobenzene chloride, can also inhibit platelet ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J63/00
Inventor 卢定强张淑敏王俊凌岫泉洪声梁铭鑫
Owner NANJING TECH UNIV
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