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Method for extraction of bilirubin from bile

A technology for bilirubin and bile, applied in the direction of organic chemistry and the like, can solve the problems of low yield, cumbersome process, low purity, etc., and achieve the effect of improving the purity and increasing the adsorption effect.

Inactive Publication Date: 2015-08-12
TIANYIYANG TIANJIN BIO SEPARATION ENG TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Bilirubin is mainly extracted from bile. Bilirubin is insoluble in water, soluble in organic solvents such as stupid, chloroform and carbon disulfide, slightly soluble in ethanol and ether, and also soluble in hot ethanol and chloroform mixture. Among them, the sodium salt of bilirubin is easily soluble in water, but calcium salt, magnesium salt, barium salt, etc. are insoluble in water; bilirubin is mostly made of fresh pig bile through quicklime to generate bilirubin calcium salt, and then hydrochloric acid Forget it, it is obtained by chloroform solvent extraction, but the process is cumbersome, the yield is low, only about 0.02-0.04%, and the purity is also low, only 60-70%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1 A method for extracting bilirubin from bile, including the following steps:

[0016] (1) Hydrolysis treatment: Take 1000g of fresh pig bile, add 2g of sodium bisulfite and ammonium sulfate for hydrolysis for 3h;

[0017] (2) Adsorption treatment: At a temperature of 50°C, add 20 g of polyacrylate resin to the hydrolyzed solution in step (1) for adsorption for 4 hours;

[0018] (3) Washing treatment: Wash the adsorbed resin 3 times with a mixture of ethanol and chloroform with a hot molar ratio of 5:1, continue to add a small amount of sodium bisulfite to the washing solution, let it stand for 30 minutes, and then The obtained mixture was washed 5 times with a small amount of slightly hot 95% ethanol and distilled water;

[0019] (4) Vacuum drying treatment: the filtrate is dried and crystallized under reduced pressure at a temperature of 10°C to obtain bilirubin crystal particles. The yield of the final product is 0.05% and the purity is 99%.

Embodiment 2

[0020] Example 2 A method for extracting bilirubin from bile, including the following steps:

[0021] (1) Hydrolysis treatment: Take 1000g of fresh pig bile and add 1.8g of sodium bisulfite and ammonium sulfate for hydrolysis for 5h;

[0022] (2) Adsorption treatment: Add 30 g of polyacrylate resin to the hydrolyzed solution in step (1) for 4 hours of adsorption at a temperature of 50°C;

[0023] (3) Washing treatment: Wash the resin after adsorption treatment with a mixture of ethanol and chloroform with a hot molar ratio of 8:1 for 5 times, continue to add a small amount of sodium bisulfite to the washing solution, let it stand for 30 minutes, and then The obtained mixture was washed 3 times with a small amount of slightly hot 95% ethanol and distilled water;

[0024] (4) Vacuum drying treatment: the filtrate is dried and crystallized under reduced pressure at a temperature of 10°C to obtain bilirubin crystal particles. The yield of the final product is 0.052% and the purity is 99%...

Embodiment 3

[0025] Example 3 A method for extracting bilirubin from bile, including the following steps:

[0026] (1) Hydrolysis treatment: Take 1000g of fresh pig bile, add 1.5g of sodium bisulfite and ammonium sulfate for hydrolysis for 8h;

[0027] (2) Adsorption treatment: At a temperature of 60°C, add 10 g of polyacrylate resin to the hydrolyzed solution in step (1) for adsorption for 3 hours;

[0028] (3) Washing treatment: Wash the adsorbed resin 3 times with a mixture of ethanol and chloroform with a hot molar ratio of 8:1, continue to add a small amount of sodium bisulfite to the washing solution, let stand for 30 minutes, and then The obtained mixture was washed 3 times with a small amount of slightly hot 95% ethanol and distilled water;

[0029] (4) Vacuum drying treatment: the filtrate is dried and crystallized under reduced pressure at a temperature of 20°C to obtain bilirubin crystal particles. The yield of the final product was 0.05%, and the purity was 98.6%.

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PUM

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Abstract

The invention provides a method for extraction of bilirubin from bile. The method includes: firstly taking fresh pig bile, adding sodium bisulfite and ammonium sulfate to conduct hydrolysis for 3-8h; then adding a certain amount of macroporous resin into the hydrolysate to conduct adsorption for 2-4h; then washing the resin subjected to adsorption treatment with a hot ethanol-chloroform mixed solution repeatedly, further adding a small amount of sodium bisulfite into the washing solution, conducting standing for 10-30min, and flushing the obtained mixture with a small amount of tepid 95% ethanol and distilled water repeatedly; and finally subjecting the filtrate to vacuum drying and crystallization, thus obtaining bilirubin crystal grains. The method provided by the invention utilizes the adsorption effect of macroporous resin to extract bilirubin and has no damage to bilirubin, the process is simple, and the extracted bilirubin product has high yield and high purity.

Description

Technical field [0001] The invention relates to the technical field of bilirubin extraction, in particular to a method for extracting bilirubin from bile. Background technique [0002] Bilirubin is mainly extracted from bile. Bilirubin is insoluble in water, soluble in organic solvents such as benzene, chloroform and carbon disulfide, slightly soluble in ethanol and ether, and also soluble in a mixture of hot ethanol and chloroform Among them, the sodium salt of bilirubin is easily soluble in water, but calcium salt, magnesium salt, barium salt, etc. are insoluble in water; bilirubin is mostly produced from fresh pig bile through the action of quicklime to generate bilirubin calcium salt, and then hydrochloric acid After all, it is prepared by chloroform solvent extraction, but the process is complicated, the yield is low, only about 0.02-0.04%, and the purity is also low, only 60-70%. Summary of the invention [0003] In order to solve the above technical problems, the technical...

Claims

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Application Information

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IPC IPC(8): C07D207/44
CPCC07D207/44
Inventor 欧阳玉岭
Owner TIANYIYANG TIANJIN BIO SEPARATION ENG TECH CO LTD
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