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Method for purifying ursodeoxycholic acid by mixed solvent

A technology of ursodeoxycholic acid and mixed solvent, applied in the field of medicine, can solve the problems of high yield of ursodeoxycholic acid, high energy consumption of solvent recovery, small solvent consumption, etc. The effect of increasing production efficiency

Inactive Publication Date: 2010-07-21
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to propose a method for purifying ursodeoxycholic acid with a mixed solvent in view of problems such as low solubility, large solvent consumption, and large energy consumption for solvent recovery when using ethyl acetate to purify ursodeoxycholic acid in current industrial production , with the characteristics of low solvent consumption and high yield of ursodeoxycholic acid

Method used

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  • Method for purifying ursodeoxycholic acid by mixed solvent

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Experimental program
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Effect test

Embodiment 1

[0011] Get ethanol 0.5kg, ethyl acetate 9.5kg, mix and make the mixed solvent that weight ratio is 5:95. Take 1 kg of cholic acid mixture to be purified, the purity of ursodeoxycholic acid is 60% by mass fraction, add 1.6 kg of mixed solvent at one time, stir for 1 h, and then keep it sealed for 20 h. Filtration gave an insoluble solid. The insoluble solid was dried to obtain 0.56 kg of ursodeoxycholic acid product. The purity of the ursodeoxycholic acid product was determined by high performance liquid chromatography, and it was 95.3% in terms of mass fraction.

[0012] The chromatographic condition that high performance liquid chromatography measures ursodeoxycholic acid product purity is:

[0013] The column is Dima C 18 Column (250mm×4.6mm i.d., 5μm), the mobile phase is 0.2% acetic acid acetonitrile-0.2% acetic acid water (70:30), the flow rate is 1.0mL / min, the column temperature is 30°C, and the injection volume is 10μL; : Evaporative light scattering detector (ELSD...

Embodiment 2

[0018] Get n-propanol 1kg, ethyl acetate 9kg, mix and make the mixed solvent that weight ratio is 1:9. Take 1 kg of cholic acid mixture to be purified, and its ursodeoxycholic acid purity is 70% in terms of mass fraction. Add 0.8 kg of mixed solvent for washing, stir for 1 h, then seal and let stand for 5 h, filter, and wash the insoluble solid again once more. The insoluble solid was dried to obtain 0.65 kg of ursodeoxycholic acid product, and the purity of the ursodeoxycholic acid product was determined according to the high performance liquid chromatography conditions of Example 1, and it was 96.3% in mass fraction.

Embodiment 3

[0020] Get isopropanol 2kg, isopropyl acetate 8kg, mix and make the mixed solvent that weight ratio is 2:8. Take 1 kg of the cholic acid mixture to be purified, and its ursodeoxycholic acid purity is 55% by mass fraction. Add 0.4kg of mixed solvent to dissolve, stir for 1 hour, then seal and let stand for 5 hours, then filter to obtain insoluble solid. The above washing process was repeated 4 times. The insoluble solid was dried to obtain 0.48 kg of ursodeoxycholic acid product, and the purity of the ursodeoxycholic acid product was determined according to the high performance liquid chromatography conditions of Example 1, and it was 97.6% by mass fraction.

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Abstract

The invention provides a method for purifying ursodeoxycholic acid by a mixed solvent, which comprises three steps of preparing the mixed solvent, washing a cholic acid mixture and drying to obtain the ursodeoxycholic acid. The method is characterized by using the mixed solvent prepared from 1-80 parts of small molecule alcohol and 99-20 parts of small molecule ester by weight. The mixed solvent can selectively dissolve impurities of chenodeoxycholic acid, and the like in the cholic acid mixture and reserve the ursodeoxycholic acid. The mixed solvent not only reserves strong dissolving capacity of alcohol on the chenodeoxycholic acid, but also reserves the characteristic of ester for selectively dissolving the chenodeoxycholic acid. Under the premise of the same production capacity, the method for purifying the ursodeoxycholic acid of the invention can obviously reduce the consumption of organic solvent, saves the energy consumption of solvent recovery, and is suitable for preparing high purity ursodeoxycholic acid.

Description

technical field [0001] The invention belongs to a separation method in the field of medicine, in particular to a method for purifying ursodeoxycholic acid with a mixed solvent. Background technique [0002] Ursodeoxycholic acid (3α, 7β-dihydroxy-5β-cholic acid, Ursodeoxycholic Acid) is a dihydroxycholic acid, which accounts for about 3% of the total human bile. Ursodeoxycholic acid is a non-toxic hydrophilic bile acid that has therapeutic effects on many diseases. Currently, ursodeoxycholic acid is used in the treatment of primary sclerosing cholangitis, cholesterol gallstones, bile reflux gastritis and biliary pancreatitis. In addition, ursodeoxycholic acid is the drug of choice for cholestatic liver disease and is used to improve survival after liver transplantation. [0003] Ursodeoxycholic acid is a bile acid component unique to bears, and it is mainly obtained by two methods at present. The first is to breed bears, then obtain bear bile through in vivo drainage, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
Inventor 龚行楚瞿海斌程翼宇王珏
Owner ZHEJIANG UNIV
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