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Method for extracting hyodeoxycholic acid from pig gall paste

A technology of hyodeoxycholic acid and pig bile ointment is applied in the directions of steroids, organic chemistry, etc., and can solve the problems of hyodeoxycholic acid having a great influence on the quality, complicated extraction method operation, affecting environmental quality and the like, and achieving low cost, Simple preparation steps and the effect of avoiding contamination

Active Publication Date: 2022-04-12
福建省南仹生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the traditional extraction method of hyodeoxycholic acid, a large amount of organic solvent ethyl acetate is used for extraction and then decolorized with activated carbon. However, due to the volatility of the organic solvent ethyl acetate, it is easy to decompose when heated. The quality of the acid has a great influence; and the traditional extraction method is complicated to operate and the production cost is high; at the same time, the volatilization of ethyl acetate will affect the environmental quality.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A method for extracting hyodeoxycholic acid from pig gall paste, comprising the following steps:

[0037] Step 1: Add sodium hydroxide and water to the pig gall paste, raise the temperature to 100°C, stir and reflux for 20 hours, let stand and cool to room temperature, and remove the upper solution;

[0038] Step 2, adjusting the pH of the lower layer solution obtained in Step 1 to 8.2, adding magnesium salt, stirring and crystallizing for 6 hours, filtering, and collecting the solid;

[0039] Step 3, adding water to the solid collected in Step 2, heating to 40°C, adding an acidic solution to adjust the pH to 6.2, stirring and filtering to obtain the crude product;

[0040] Step 4: Add water, sodium carbonate, and activated carbon to the crude product obtained in Step 3, stir, heat to 90°C, reflux for 1 hour, let stand at room temperature, and collect the filtrate;

[0041] Step five, adjust the pH of the filtrate obtained in step four to 3.3, press filter, then wash w...

Embodiment 2

[0049] A method for extracting hyodeoxycholic acid from pig gall paste, comprising the following steps:

[0050] Step 1, add sodium hydroxide and water to the pig gall paste, raise the temperature to 110°C, stir and reflux for 18h, let stand and cool to room temperature, and remove the upper solution;

[0051] Step 2, adjust the pH of the lower layer solution obtained in Step 1 to 8.3, add magnesium salt, stir and crystallize for 4 hours, filter, and collect the solid;

[0052] Step 3, adding water to the solid collected in Step 2, heating to 50°C, adding an acidic solution to adjust the pH to 6.3, stirring and filtering to obtain the crude product;

[0053] Step 4: Add water, sodium carbonate, and activated carbon to the crude product obtained in Step 3, stir, heat to 100°C, reflux for 1 hour, let stand at room temperature, and collect the filtrate;

[0054] Step 5: Adjust the pH of the filtrate obtained in Step 4 to 3.4, press filter, then wash with sodium bicarbonate solut...

Embodiment 3

[0062] A method for extracting hyodeoxycholic acid from pig gall paste, comprising the following steps:

[0063] Step 1: Add sodium hydroxide and water to the pig gall paste, raise the temperature to 105°C, stir and reflux for 19 hours, let stand and cool to room temperature, and remove the upper solution;

[0064] Step 2, adjust the pH of the lower layer solution obtained in Step 1 to 8.2, add magnesium salt, stir and crystallize for 5 hours, filter, and collect the solid;

[0065] Step 3, adding water to the solid collected in Step 2, heating to 45°C, adding an acidic solution to adjust the pH to 6.3, stirring and filtering to obtain the crude product;

[0066] Step 4: Add water, sodium carbonate, and activated carbon to the crude product obtained in Step 3, stir, heat to 95°C, reflux for 1 hour, let stand to room temperature, and collect the filtrate;

[0067] Step five, adjust the pH of the filtrate obtained in step four to 3.3, press filter, then wash with sodium bicarbo...

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Abstract

A method for extracting hyodeoxycholic acid from pig gall paste comprises the following steps: step 1, adding sodium hydroxide and water into the pig gall paste, heating to 100-110 DEG C, stirring and refluxing for 18-20 hours, standing and cooling to room temperature, and removing an upper solution; 2, adjusting the pH value of the lower-layer solution obtained in the step 1 to 8.2-8.3, adding magnesium salt, stirring and crystallizing for 4-6 hours, filtering, and collecting a solid; step 3, adding water into the solid collected in the step 2, heating to 40-50 DEG C, adding an acidic solution to adjust the pH to 6.2-6.3, stirring, and filtering to obtain a crude product; step 4, adding water and sodium carbonate into the crude product prepared in the step 3, stirring, heating to 90-100 DEG C, refluxing for 1 hour, standing to room temperature, and collecting filtrate; and 5, adjusting the pH value of the filtrate obtained in the step 4 to 3.3-3.4, carrying out filter pressing, washing with a sodium bicarbonate solution until the pH value is 6.5-6.6, drying, and crushing to obtain the hyodeoxycholic acid. The yield of the hyodeoxycholic acid prepared by the method is up to 35%, the melting point is 200 DEG C, the preparation steps are simple, no organic solvent is adopted for extraction, and the cost is low.

Description

technical field [0001] The invention belongs to the field of preparation of hyodeoxycholic acid, in particular to a method for extracting hyodeoxycholic acid from pig gall paste. Background technique [0002] Hyodeoxycholic acid (HDCA) is a blood lipid-lowering drug that can inhibit the formation of cholic acid and dissolve fat, reduce blood cholesterol and triglycerides, and is suitable for type Ia or Ib hyperlipidemia and atherosclerosis. Hyodeoxycholic acid is an important raw material of artificial bezoar formula, and hyodeoxycholic acid with a purity of ≥99.0% is required in actual production. In the traditional extraction method of hyodeoxycholic acid, a large amount of organic solvent ethyl acetate is used for extraction and then decolorized with activated carbon. However, due to the volatility of the organic solvent ethyl acetate, it is easy to decompose when heated. The quality of the acid has a great influence; and the traditional extraction method is complicated ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
CPCY02P20/10
Inventor 林夏楠彭秋生鲍涵铸
Owner 福建省南仹生物科技有限公司
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