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Purification method for removing 22-ene-UDCA impurity in ursodesoxycholic acid

A technology of 22-ene-udca and ursodeoxycholic acid, which is applied in the field of purification to remove 22-ene-UDCA impurities in ursodeoxycholic acid, and can solve the problem that the pharmaceutical effect of ursodeoxycholic acid is affected and the impurities are not good The removal method and other issues, to achieve the effect of low cost, convenient operation, and thorough purification reaction

Pending Publication Date: 2022-04-12
CHANGDE YUNGANG BIOTECHNOLOGY CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] 22-ene-UDCA cannot be detected by high performance liquid chromatography, and its position can only be detected by ultraviolet liquid chromatography. This substance has a large absorption coefficient in ultraviolet light, and the peak position is close to UDCA. Currently, there is no such impurity A better removal method, in view of the fact that the appearance of the impurity 22-ene-UDCA will have a certain impact on the pharmaceutical effect of ursodeoxycholic acid, therefore, how to effectively remove the impurity 22-ene-UDCA in ursodeoxycholic acid , which has great significance in the field of medicine

Method used

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  • Purification method for removing 22-ene-UDCA impurity in ursodesoxycholic acid
  • Purification method for removing 22-ene-UDCA impurity in ursodesoxycholic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Take 100g of ursodeoxycholic acid and pour it into a 2000ml flask, dissolve it in a solvent mixed with 800ml of n-butanol and 50ml of water, stir and dissolve it in an oil bath at 60°C; add 50g of potassium hydroxide solid to the flask , Distill under reduced pressure in a vacuum of 20kp, azeotropically distill for 20 minutes, remove the water in the solvent, and take a sample to determine that the residual water content of the solvent is about 0.3%; , stirred and reacted for 8 hours, terminated the reaction, thoroughly recovered the solvent by distillation under reduced pressure, added hydrochloric acid to adjust the pH value to 2-3, filtered with suction, separated, collected the solid in a decompression drying box, and detected it with ultraviolet liquid phase, and obtained no Ursodeoxycholic acid containing 22-ene-UDCA 98.4g.

Embodiment example 2

[0031] Take 100g of ursodeoxycholic acid and pour it into a 2000ml flask, and dissolve it in a solvent mixed with 1000ml of n-amyl alcohol and 90ml of water, stir and dissolve in an oil bath at 70°C; add 70g of potassium hydroxide solid to the flask, Distill under reduced pressure at a vacuum of 20kp, azeotropically distill for 20 minutes, remove the water in the solvent, and take a sample to determine that the residual water content of the solvent is about 0.2%; pour the solvent into a flask, place in an oil bath at 120°C, Stir the reaction for 9 hours, terminate the reaction, distill the solvent under reduced pressure and recover thoroughly, add hydrochloric acid to adjust the pH value to 2-3, filter with suction, separate, collect the solid in a decompression drying box, and detect it with ultraviolet liquid phase, and obtain 22-ene-UDCA ursodeoxycholic acid 98.7g.

Embodiment example 3

[0033] Get 100g of ursodeoxycholic acid and pour it into a 2000ml flask, and dissolve it in a solvent mixed with 1200ml of n-hexanol and 90ml of water, stir and dissolve in an oil bath at 80°C; add 80g of potassium hydroxide solid to the flask, Distill under reduced pressure at a vacuum of 20kp, azeotropically distill for 20 minutes, remove the water in the solvent, and take a sample to determine that the residual water content of the solvent is about 0.2%, pour the solvent into a flask, and stir in an oil bath at 130°C After reacting for 10 hours, the reaction was terminated, the solvent was distilled under reduced pressure and recovered thoroughly, hydrochloric acid was added to adjust the pH value to 2-3, suction filtration, separation, the solid was collected and placed in a decompression drying oven, and detected by ultraviolet liquid phase, the obtained 22-free -ene-UDCA ursodeoxycholic acid 98.5g.

[0034] It can be seen from the above examples that in the purification ...

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Abstract

The invention discloses a purification method for removing 22-ene-UDCA impurities in ursodesoxycholic acid. The purification method comprises the following process steps: dissolving ursodesoxycholic acid, adding potassium hydroxide solid into a dissolving agent, removing water in a solvent to obtain a water removal system, refluxing the water removal system, carrying out reduced pressure distillation to recover the solvent, acidifying, separating and the like. The purification method provided by the invention only needs one solvent, is easy to recover, convenient to operate and low in solvent toxicity, and can effectively remove the impurity 22-ene-UDCA of the ursodesoxycholic acid.

Description

technical field [0001] The invention relates to the technical field of purification of ursodeoxycholic acid, in particular to a purification method for removing 22-ene-UDCA impurities in ursodeoxycholic acid. Background technique [0002] Ursodeoxycholic acid (3a,7β-dihydroxy-5β-cholestane-24-acid) referred to as UDCA is odorless, bitter, soluble in ethanol, insoluble in chloroform. Ursodeoxycholic acid is the main component of traditional Chinese medicine bear bile. It can promote the secretion of endogenous bile acids, reduce reabsorption, and antagonize the cytotoxicity of hydrophobic bile acids. It can protect liver cell membranes, dissolve cholesterol gallstones, and Immunomodulatory role. The current ursodeoxycholic acid basically contains impurities mainly composed of cholic acid and allochodeoxycholic acid, and high-purity ursodeoxycholic acid is the basis of clinical medicine, and purified ursodeoxycholic acid can be better To provide precise research for its medi...

Claims

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Application Information

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IPC IPC(8): C07J9/00
Inventor 邓家国万里平李国军谢小国唐雪文盛敏李跃忠曾飞洪媛
Owner CHANGDE YUNGANG BIOTECHNOLOGY CO LTD
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