A kind of separation method of chenodeoxycholic acid and ursodeoxycholic acid

A technology of ursodeoxycholic acid and chenodeoxycholic acid, which is applied in the field of biochemical separation, can solve the problems of low unit solvent production capacity, large solvent consumption, and low product yield, and achieve good separation and purification performance and industrial production The effect of high efficiency and low production cost

Active Publication Date: 2011-12-21
上海华震科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the solvent method has the disadvantages of low production capacity per unit solvent, large solvent consumption, high solvent toxicity, and low product yield.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Dissolve a mixture containing 4.5g of ursodeoxycholic acid and 6g of chenodeoxycholic acid in an aqueous sodium hydroxide solution, adjust the pH to 8, add 75ml of deionized water to dilute to form an upper column liquid; pass the upper column liquid through The peristaltic pump is injected into the resin column filled with the non-polar porous synthetic adsorbent macroporous adsorption resin HZ816, and then the first eluent configured with three times the column volume (600ml) of 30% methanol aqueous solution is pumped into the adsorption resin The column is desorbed, the eluent is eluted at a flow rate of 1 column volume / hour (200ml / h), and the eluents (mainly ursodeoxycholic acid sodium salt in the eluent) are collected and doubled The column volume (400ml) of pure methanol solution is configured as the second eluent, pumped into the adsorption resin column for desorption, the elution flow rate is 1 column volume / hour (200ml / h), and the obtained eluent (solution (Main...

Embodiment 2

[0028] Except that the non-polar macroporous adsorption resin HZ818 was used to replace HZ816 in Example 1, the other operations were the same as in Example 1. The result was determined that the content of ursodeoxycholic acid in the 30% methanol eluate was 82.2% by mass fraction. , The content of chenodeoxycholic acid is 17.8%. In the pure methanol eluate, the content of ursodeoxycholic acid is 12.8% and the content of chenodeoxycholic acid is 87.2% in terms of mass fraction. The total recovery rate of ursodeoxycholic acid was 82%, and that of chenodeoxycholic acid was 83%.

Embodiment 3

[0030] The non-polar macroporous adsorption resin HZ830 was used to replace HZ816 in Example 1, and the other conditions were the same as in Example 1. The result was determined that the content of ursodeoxycholic acid in the 30% methanol eluate was 83.2% by mass fraction. The content of deoxycholic acid was 16.8%. In the pure methanol eluate, in terms of mass fraction, the content of ursodeoxycholic acid was 12.3% and the content of chenodeoxycholic acid was 87.7%. The total recovery rate of ursodeoxycholic acid was 85%, and that of chenodeoxycholic acid was 81%.

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Abstract

The invention discloses a method for separating chenodeoxycholic acid from ursodesoxycholic acid, which belongs to the technical field of biochemical separation and is characterized by comprising the following steps in turn: (1) preparing column loading solution, namely dissolving mixture of ursodesoxycholic acid and chenodeoxycholic acid in alkaline aqueous solution according an equivalence ratio of 1:2.5, regulating the pH value of the solution to 7 to 8, and diluting deionized water till the solid content is 10 to 20 percent; (2) loading onto a column for absorption, namely pumping the column loading solution into a resin column filled with nonpolar porous synthetic absorbent; (3) desorbing, namely preparing eluting solution by using water soluble organic solvent, and pumping the eluting solution into the resin column for desorbing; and (4) performing post-treatment, namely concentrating under vacuum, recovering solvent, adding acid solution into the concentrated product to regulate the pH value to 2 to 3, precipitating, filtering, washing till the pH value is 7, drying, crystallizing and drying under vacuum to obtain a finished product. The method has the advantages that: the macroporous resin has high separation and purification performance and high accuracy; the ursodesoxycholic acid is separated from chenodeoxycholic acid with high yield; the process is simple; the production cost is low; and the industrial production efficiency is high.

Description

Technical field [0001] The invention relates to a method for separating chenodeoxycholic acid and ursodeoxycholic acid, in particular to a method for separating chenodeoxycholic acid and ursodeoxycholic acid by using a macroporous adsorption resin, and belongs to the technical field of biochemical separation . Background technique [0002] Ursodeoxycholic acid is a non-toxic hydrophilic cholic acid, which has therapeutic effects on many diseases. Ursodeoxycholic acid is currently used for the treatment of diseases such as primary sclerosing cholangitis, cholesterol gallstones, bile reflux gastritis and biliary pancreatitis. In addition, ursodeoxycholic acid is also the drug of choice for cholestatic liver disease and is used to increase the survival rate after liver transplantation. [0003] Ursodeoxycholic acid is a bile acid component unique to bears, and its structural formula is shown in general formula (1): [0004] ⑴ [0005] At present, ursodeoxycholic aci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
Inventor 江邦和厉留柱宁方红徐环昕李大芦
Owner 上海华震科技有限公司
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