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Method for purifying chenodeoxycholic acid

A technology of chenodeoxycholic acid and a purification method, which is applied in the field of purifying chenodeoxycholic acid to achieve the effects of low organic residue, easy standardization, and large-scale industrial production

Inactive Publication Date: 2015-01-28
SHANGHAI FENPU NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Current literature reports on methods for separating chenodeoxycholic acid from animal bile, focusing on solvent extraction, precipitation, silica gel chromatography, and ion exchange resin methods , macroporous resin method and other methods, such as: what Chinese patent CN1775798 adopted was ion exchange method, what Chinese patent CN101143886, CN103113447A and Chinese patent CN101948496A adopted was precipitation method, what Chinese patent CN 102703556A adopted was macroporous resin method etc., these methods There are disadvantages such as complicated separation process, low yield, low product purity, poor reproducibility, long time consumption, serious organic residues, and incapability of large-scale production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Quantitatively weigh 1 kg of commercially available pig gall paste, put it in a 10-liter extraction tank, add 5 liters of petroleum ether, heat to 60 ° C and reflux for 3 hours, remove the petroleum ether, and repeat this operation once more to obtain crude oil that has been degreased. Gallbladder paste 850g, the 850g crude gallbladder paste was added to 5L ethyl acetate to reflux to dissolve, then add 85g activated carbon to decolorize and reflux at 80°C for 2 hours, then filter to remove activated carbon, then remove ethyl acetate to obtain decolorized and degreased pig gallbladder Paste 841g, this 841g crude bile paste is dissolved in the mass fraction of 4.2kg in the sodium hydroxide aqueous solution of 1%, the pH of adjustment solution is 8, uses the microfiltration membrane of 0.45 μm pore size, the ultrafiltration membrane of 0.01 μm pore size successively Remove suspended colloidal particle impurities by filtration to obtain clear components to be chromatographic...

Embodiment 2

[0036] Quantitatively weigh 1 kg of commercially available pig gall paste, put it in a 10-liter extraction tank, add 3.8 liters of cyclohexane and heat it to reflux at 80°C for 3 hours, remove the cyclohexane, and repeat this operation 2 more times to obtain degreased Crude gall paste 855g, this 855g thick gall paste is added 5L ethanol reflux dissolving, add 85g gac again after fully dissolving and take off reflux for 2 hours, filter and remove gac, then remove ethanol, obtain the decolorized degreasing thick gall paste 842g, this 842g rough Dissolve 4.2kg of 1% sodium hydroxide aqueous solution in the gall paste, adjust the pH of the solution to 9, and remove the suspended colloidal particle impurities by successively filtering with a microfiltration membrane with a pore size of 0.45 μm and an ultrafiltration membrane with a pore size of 0.01 μm Obtain clear components to be chromatographically separated;

[0037] Take an industrial chromatographic column with a column lengt...

Embodiment 3

[0039] Quantitatively weigh 1 kg of commercially available pig gall powder, put it in a 10-liter extraction tank, add 4.2 liters of n-hexane and heat it to reflux at 65°C for 3 hours, remove the n-hexane, and repeat this operation once more to obtain fat-free gallbladder Powder 845g, add 7.6L chloroform reflux and dissolve this 845g coarse gall powder, add 85g gac after fully dissolving and take off reflux for 2 hours, filter and remove gac, remove chloroform again, get decolorized degreasing coarse gall powder 831g, this 831g coarse gall powder Dissolve the powder in 4.2 kg of 1% sodium hydroxide aqueous solution, and then filter through a microfiltration membrane with a pore size of 0.45 μm and an ultrafiltration membrane with a pore size of 0.01 μm to remove the suspended colloidal particle impurities to obtain a clear component to be chromatographically separated ;

[0040] Take an industrial chromatographic column with a column length of 600 mm and an inner diameter of 13...

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Abstract

The invention discloses a method for purifying chenodeoxycholic acid. The method comprises the following steps: pretreatments such as degreasing, decoloration and impurity removal are carried out on commercially available crude bile paste or crude bile powder, so as to obtain a component to undergo chromatographic separation; the component to undergo chromatographic separation undergoes purification and separation by the use of a chromatographic column with a hydrophilic resin filler as a stationary phase; and separation products undergo concentration, acidification, washing and drying, so as to obtain chenodeoxycholic acid. In comparison with the prior art, the invention has the following beneficial effects: 1, content of the main component is high; 2, reappearance is high and operability is good; 3, short cycle: it only takes two days to prepare the high-purity chenodeoxycholic acid product from processing of the bile paste raw material; and 4, low content of organic residues: as processes such as solvent extraction, column chromatography on silica gel and the like in the traditional techniques are abandoned, an industrial chromatographic process with low dosage of an organic solvent is adopted and the final product undergoes drying process, the content of the residual organic solvent in the final product is especially low.

Description

technical field [0001] The invention relates to a method for purifying chenodeoxycholic acid, which belongs to the technical field of separation and purification of biomedicine. Background technique [0002] Chenodeoxycholic acid (CDCA for short), chemical name 3α, 7α-dihydroxy-5β-cholic acid, molecular formula C 24 h 4 0O 4 , with a molecular weight of 392.58, is currently one of the most widely used medicines for treating gallstones in the world, and is also the raw material for the synthesis of ursodeoxycholic acid (UDCA) and other steroidal compounds. In industry, chenodeoxycholic acid is mainly extracted from animal bile come. [0003] The current literature reports on the method of separating chenodeoxycholic acid from animal bile, focusing on solvent extraction, precipitation, silica gel chromatography, ion exchange resin method, macroporous resin method and other methods, such as: Chinese patent CN1775798 adopted Ion exchange method, what Chinese patent CN10114...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
CPCC07J9/005
Inventor 周俊峰
Owner SHANGHAI FENPU NEW MATERIAL TECH CO LTD
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