Method for removing lithocholic acid from chenodeoxycholic acid

A technique for chenodeoxycholic acid and lithocholic acid, applied in the field of chenodeoxycholic acid, can solve the problems of difficult separation of lithocholic acid, excessive lithocholic acid concentration, large loss of effective components, etc., and achieves good economic benefits and high efficiency. The effect of resource utilization, improving extraction rate and improving crystallization rate

Active Publication Date: 2016-04-13
CHANGDE YUNGANG BIOTECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problems of excessive concentration of lithocholic acid in the crude product produced by the drainage of bile from live pigs, difficulty in separating lithocholic acid, and l

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Get 217 kg of live pig drainage bile to extract the leftovers of bilirubin, put it into a 1000L stainless steel dissolution kettle, add 440 kg of water, stir and add 20 kg of sodium hydroxide, stir and raise the temperature to 50°C, and use a concentration of 10% sodium hydroxide aqueous solution to dissolve The pH value is stable at 8-9, and all the raw materials are dissolved; then filter with a bag filter to filter out the coarse residue, which is discarded and incinerated. The filtrate is bile acid sodium salt solution, and the filtrate is pumped into a 1000L enamel extraction kettle for use.

[0016] The interlayer of the extraction kettle enters the cooling water, cools the bile acid sodium salt solution to room temperature (25°C), adds 500L of n-heptane, slowly adds 10% diluted hydrochloric acid solution dropwise while stirring, and adjusts the pH to 2.5. At this time, the solution crystallizes After being turbid, the temperature was raised to a solution temperatu...

Embodiment 2

[0021] Get 207 kg of live pig drainage bile to extract the leftovers of bilirubin, put it into a 1000L stainless steel dissolution kettle, add 414 kg of water, stir and add 18 kg of sodium hydroxide, stir and raise the temperature to 50°C, and use a concentration of 10% sodium hydroxide aqueous solution to dissolve The pH value is stable at 8-9, and all the raw materials are dissolved; then filter with a bag filter to filter out the coarse residue, which is discarded and incinerated. The filtrate is bile acid sodium salt solution, and the filtrate is pumped into a 1000L enamel extraction kettle for use.

[0022] The interlayer of the extraction kettle enters the cooling water, cools the bile acid sodium salt solution to room temperature (25°C), adds 490L of n-heptane, slowly adds 10% diluted hydrochloric acid solution dropwise while stirring, and adjusts the pH to 3.0. At this time, the solution crystallizes After being turbid, the temperature was raised to a solution temperatu...

Embodiment 3

[0027] Get 229 kg of live pig drainage bile to extract the leftovers of bilirubin, put it into a 1000L stainless steel dissolution kettle, add 460 kg of water, stir and add 21 kg of sodium hydroxide, stir and raise the temperature to 50°C, and use a concentration of 10% sodium hydroxide aqueous solution to dissolve The pH value is stable at 8-9, and all the raw materials are dissolved; then filter with a bag filter to filter out the coarse residue, which is discarded and incinerated. The filtrate is bile acid sodium salt solution, and the filtrate is pumped into a 1000L enamel extraction kettle for use.

[0028]The interlayer of the extraction kettle enters the cooling water, cools the bile acid sodium salt solution to room temperature (25°C), adds 520L of n-heptane, slowly adds 10% diluted hydrochloric acid solution dropwise while stirring, and adjusts the pH to 2.8. At this time, the solution crystallizes After being turbid, the temperature was raised to a solution temperatur...

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PUM

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Abstract

The invention discloses a method for removing lithocholic acid from chenodeoxycholic acid. The method comprises steps as follows: dissolving, extraction separation, crude product drying and mother solution treatment of chenodeoxycholic acid, crystallization, drying of a finished product, leftover recycling and the like. According to the great dissolution difference of lithocholic acid, lipid-like substances and chenodeoxycholic acid in n-heptane, more than 90% of lithocholic acid and the lipid-like substances are extracted once, the operation is simple and efficient, moreover, chenodeoxycholic acid is non-loss, n-heptane has a higher boiling point and is not prone to volatilization, a butyl acetate and methylene dichloride mixed solvent is adopted for crystallization, the crystallization ratio of chenodeoxycholic acid, the dissolution rate of lithocholic acid and other hetero-cholic acid and the extraction rate of chenodeoxycholic acid are increased, biological non-renewable resources are utilized to the greatest extent, and better economic benefits and resource utilization rate are created.

Description

technical field [0001] The invention relates to the technical field of chenodeoxycholic acid, in particular to a method for removing lithocholic acid from chenodeoxycholic acid. Background technique [0002] Lithocholic acid is a kind of harmful bile acid for human and animal bodies. If the content in bile is too high, it will cause diarrhea, gastroenteritis and other digestive tract diseases. Pharmacopoeias at home and abroad have strict requirements on the concentration of lithocholic acid for the use of bile acids in medicine. Among them, the concentration of lithocholic acid in ursodeoxycholic acid raw materials must be controlled within 0.1%, and chenodeoxycholic acid is ursodeoxycholic acid Synthetic biological raw materials, so the content of lithocholic acid must be strictly controlled. [0003] The current conventional method for removing lithocholic acid is the ethyl acetate crystallization method. This method has a good removal effect on the chenodeoxycholic acid...

Claims

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Application Information

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IPC IPC(8): C07J9/00
CPCC07J9/005
Inventor 邓家国
Owner CHANGDE YUNGANG BIOTECHNOLOGY CO LTD
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