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A kind of purification method of sodium glycochenodeoxycholate

A technology of sodium glycine chenodeoxycholate and glycine chenodeoxycholic acid is applied in the purification field of sodium glycine chenodeoxycholate, which can solve the problem of high equipment requirements, low purity of sodium glycine chenodeoxycholate, and inability to Meet drug research and other issues

Active Publication Date: 2021-09-10
YAOPU SHANGHAI PHARMA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problem that the purity of sodium glycochenodeoxycholate prepared by the prior art is lower than 98%, it cannot meet the needs of drug research or even if sodium glycochenodeoxycholate with a purity greater than 98% is obtained, the requirements for equipment are relatively high, and industrialization cannot be realized The object of the present invention is to provide a purification method of sodium glycochenodeoxycholate, the purification method of the present invention has good stability, the purity of the product obtained is high, and the purity reaches more than 98%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 110

[0019] Example 1 Purification of crude product of 10 g sodium glycochenodeoxycholate

[0020] Preparation of potassium dihydrogen phosphate buffer solution: Dissolve 3.4 g of potassium dihydrogen phosphate in 1 L of pure water, add 2 mol / L sodium hydroxide solution dropwise to adjust the pH value to 7, and then use phosphoric acid to adjust the pH value to 2.5.

[0021] Preparation of eluent: Take 2 L of anhydrous methanol, 333.3 mL of acetonitrile and 1 L of potassium dihydrogen phosphate buffer solution prepared above and mix and stir evenly to prepare eluent, which is ready for use.

[0022] Dissolve 10 g of glycochenodeoxycholic acid sodium salt with a purity of 95% by HPLC in 20 mL of water, adjust the pH to <2 with 6 mol / L hydrochloric acid solution, a large amount of white solid precipitates, filter, and wash the filter cake with purified water. Dry to constant weight to obtain 9.2 g of crude glycochenodeoxycholic acid, which is dissolved in 30 mL of eluent for use.

...

Embodiment 2

[0025] Example 2 Purification of crude product of 100 g sodium glycochenodeoxycholate

[0026] Preparation of potassium dihydrogen phosphate buffer solution: Dissolve 6.8g of potassium dihydrogen phosphate in 2L of pure water, add 2 mol / L sodium hydroxide solution dropwise to adjust the pH value to 7, and then adjust the pH value to 2.5 with phosphoric acid.

[0027] Preparation of eluent: 4 L of anhydrous methanol, 666.6 mL of acetonitrile and 2 L of potassium dihydrogen phosphate buffer solution prepared above were mixed and stirred evenly to prepare an eluent, which was ready for use.

[0028] Dissolve 100g of glycochenodeoxycholic acid sodium salt with an HPLC purity of 95% in 200mL of water, adjust the pH to <2 with 6 mol / L hydrochloric acid solution, a large amount of white solid precipitates, filter, wash the filter cake with purified water, and dry To a constant weight, 93.8 g of crude glycochenodeoxycholic acid was obtained, which was dissolved with 200 mL of eluent f...

Embodiment 3

[0031] Example 3 Purification of crude product of 200 g sodium glycochenodeoxycholate

[0032] Preparation of potassium dihydrogen phosphate buffer solution: Dissolve 10.2g of potassium dihydrogen phosphate in 3L of pure water, add 2mol / L sodium hydroxide solution dropwise to adjust the pH value to 7, and then adjust the pH value to 2.5 with phosphoric acid.

[0033] Preparation of eluent: 6L of anhydrous methanol, 1L of acetonitrile and 3L of potassium dihydrogen phosphate buffer solution prepared above were mixed and stirred evenly to prepare eluent, which was ready for use.

[0034] Dissolve 200 g of glycochenodeoxycholic acid sodium salt with an HPLC purity of 95% in 400 mL of water, adjust the pH to <2 with 6 mol / L hydrochloric acid solution, a large amount of white solids precipitate, filter, wash the filter cake with purified water, and dry to Constant weight was obtained to obtain 182 g of crude glycochenodeoxycholic acid, which was dissolved with 360 mL of eluent for ...

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Abstract

The invention discloses a method for purifying sodium glycochenodeoxycholate, comprising the following steps: S1, dissolving crude sodium glycochenodeoxycholate in an inorganic acid solution, filtering, washing with water, and drying to obtain glycochenodeoxycholate Crude cholic acid; S2, dissolving the crude glycochenodeoxycholic acid obtained in S1 in an eluent to obtain a crude glycochenodeoxycholic acid solution. Composed of potassium hydrogen buffer solution and acetonitrile; S3, put the crude glycochenodeoxycholic acid solution obtained in S2 on the chromatography column, elute, collect the glycochenodeoxycholic acid eluent with a purity >98% detected by HPLC, concentrate, Washing with water and drying; S4, dissolving the dried product of S3 in a solvent, adding sodium hydroxide solution, and concentrating to obtain glycochenodeoxycholic acid sodium salt with a purity >98% as detected by HPLC. The purification method of the present invention is simple in operation, stable and reliable, and can prepare sodium glycochenodeoxycholate with a purity greater than 98% in large quantities.

Description

technical field [0001] The invention relates to the technical field of separation and purification of organic chemistry, in particular to a purification method of sodium glycochenodeoxycholate. Background technique [0002] Sodium glycochenodeoxycholate, a bile salt, is mainly used in biochemical research at present, and can be used as lipase accelerator, anion remover and preparation of bacterial culture medium, etc. In recent years, scientists have discovered that sodium glycochenodeoxycholate is not only a natural regulator involved in the absorption of dietary lipids and fat-soluble nutrients, but also an important signaling molecule in the human body, involved in multiple paracrine and Endocrine functions, related to the balance of lipid and cholesterol levels, control of energy expenditure and regulation of the immune system. For example, sodium glycochenodeoxycholate has a strong apoptosis-inducing effect on liver cancer cells, and can be used in biochemical and ther...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J41/00
CPCC07J41/0061
Inventor 何秀君
Owner YAOPU SHANGHAI PHARMA TECH CO LTD
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