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Chenodeoxycholic acid butyl acetate extracting solution and preparation method thereof, and preparation method of chenodeoxycholic acid ammonium salt and chenodeoxycholic acid

The technology of butyl oxycholate acetate and chenodeoxycholic acid is applied in the field of pharmaceutical preparations, and can solve the problems of long production cycle and complicated preparation method, and achieve the effects of low cost, simple preparation process and good impurity removal effect.

Pending Publication Date: 2020-12-11
四川澄华生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention provides a preparation method of chenodeoxycholic acid, which is used to solve the technical problems in the prior art: the preparation method is complex and the production cycle is long in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] A preparation method of chenodeoxycholic acid sec-butylamine salt, comprising the following steps:

[0040] S1 preparation of decolorization solution

[0041] Weigh 20g of sodium hydroxide and dissolve it in 200g of water, and add 150g of chicken gall paste (wherein the content of cholic acid is 25%). Raise the temperature to above 70°C and stir until the gall paste is completely dissolved. After the system was completely dissolved, the system was cooled down to an internal temperature of 40°C. 320ml (282g) of butyl acetate was added, and 20g of 30% hydrogen peroxide was added dropwise. After the dropwise addition is completed, stir for 3 hours at a temperature of 20-30°C to obtain a decolorizing solution.

[0042] S2 preparation of extract

[0043] Use 60% sulfuric acid to adjust the pH of the decolorized solution obtained from S1 to 5.95-6.05. After the adjustment, stir at a temperature of 20-30° C. for 0.5 h. Stand liquid separation; separate the aqueous phase a...

Embodiment 2

[0051] A preparation method of chenodeoxycholic acid tert-butylamine salt, comprising the following steps:

[0052] S1 preparation of decolorization solution

[0053] Weigh 20g of sodium hydroxide and dissolve it in 200g of water, and add 150g of chicken gall paste (wherein the content of cholic acid is 25%). Raise the temperature to above 70°C and stir until the gall paste is completely dissolved. After the system was completely dissolved, the system was cooled down to an internal temperature of 40°C. 320ml (282g) of butyl acetate was added, and 20g of 30% hydrogen peroxide was added dropwise. After the dropwise addition is completed, stir for 3 hours at a temperature of 20-30°C to obtain a decolorizing solution.

[0054] S2 preparation of extract

[0055] Use 60% sulfuric acid to adjust the pH of the decolorized solution obtained from S1 to 5.95-6.05. After the adjustment, stir at a temperature of 20-30° C. for 0.5 h. Stand liquid separation; separate the aqueous phase ...

Embodiment 3

[0099] The chenodeoxycholic acid tert-butylamine salt obtained in Example 2 was added to 4 g of sodium hydroxide and dissolved in 250 ml of water, stirred and dissolved, heated to 30° C. and adjusted to pH = 4 with 60% sulfuric acid, and a slurry solid was precipitated. Gradiently increase the internal temperature to 41°C until the layers can be rapidly and clearly separated after standing still, stir for 1 hour, filter the system and wash with tap water until neutral. The obtained solid was dried in a blast drying oven, and the temperature was set at 50°C. Chenodeoxycholic acid was obtained with a content of 92.1%.

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Abstract

The invention discloses a preparation method of a chenodeoxycholic acid butyl acetate extracting solution. The method comprises the following steps: dissolving bile paste in a sodium hydroxide aqueoussolution, adding butyl acetate and hydrogen peroxide, and stirring to obtain a decolorizing solution; taking the decolorized solution, adjusting the pH value to 5.90-6.10, standing for liquid separation, and taking an organic phase to obtain a chenodeoxycholic acid extracting liquid; adding a sodium hydroxide aqueous solution into the chenodeoxycholic acid extracting solution, standing for liquidseparation, and taking an organic layer to obtain an impurity washing solution; and adding a sodium hydroxide aqueous solution into the impurity washing solution, standing for liquid separation, andtaking an organic layer to obtain a chenodeoxycholic acid butyl acetate extracting solution. According to the invention, the purity of the chenodeoxycholic acid tert-butyl ammonium salt obtained through the preparation method is high, and chenodeoxycholic acid is further prepared through the chenodeoxycholic acid tert-butyl ammonium salt with the high purity, so that the purity of the product canbe improved, the income of enterprises can be increased, and the preparation method is simple, easy to operate and suitable for large-scale production of the enterprises.

Description

technical field [0001] The invention relates to the technical field of pharmaceutical preparations, in particular to a chenodeoxycholic acid butyl acetate extract and a preparation method, and a preparation method of chenodeoxycholic acid ammonium salt and chenodeoxycholic acid. Background technique [0002] Chenodeoxycholic acid is mainly extracted or semi-synthesized from animal bile. The animal is mainly selected from chicken, goose, pig and / or duck gallbladder. Chenodeoxycholic acid has the effect of reducing the saturation of cholesterol in the bile, thereby affecting the gallbladder Stone disease has a good therapeutic effect, chenodeoxycholic acid is also an important raw material for the chemical synthesis of ursodeoxycholic acid, and ursodeoxycholic acid is the main active ingredient of bear bile, which is effective for many diseases such as liver and gallbladder. There is a definite curative effect. [0003] There are many technical problems in the existing prepar...

Claims

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Application Information

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IPC IPC(8): C07J9/00
CPCC07J9/005
Inventor 向世明董强黄显袁伟黄松周彩娥张翔黄清东邓治荣刘金凤宋立波
Owner 四川澄华生物科技有限公司
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