Preparation method of high-purity hyodeoxycholic acid

Abstract

The invention discloses a preparation method of high-purity hyodeoxycholic acid. The preparation method comprises the steps: weighing raw materials, adding strong alkaline and water, saponifying at the temperature of 95-100 DEG C for 16-24h, cooling to room temperature, standing, siphoning to remove a supernatant liquid, adding water into paste in the lower layer, stirring for dissolving the paste, adding strong acid to acidize until a congo red test paper turns to be blue, adding ethyl acetate, stirring for extracting for 20-50min, standing for layering, removing a water phase, adding water into the ethyl acetate to wash until the pH value of the water phase is equal to 6-7, adding the ethyl acetate into anhydrous sodium sulfate to dehydrate, carrying out activated carbon decoloration, filtering, concentrating until precipitates are separated out, cooling, filtering or squeezing and drying in vacuum; adding an alcohol solvent, stirring for dissolving the above product, slowly adding an alkaline organic solvent, stirring, cooling, separating out a great number of precipitates, filtering and drying; and adding water and sodium hydroxide, stirring for dissolving, dropwise adding hydrochloric acid with a volume concentration of 1:1, stirring, filtering and drying to obtain the hyodeoxycholic acid. The invention aims to provide the preparation method of the hyodeoxycholic acid with simple process, high yield and high purity.

Description

technical field [0001] The invention relates to a preparation method of high-purity hyodeoxycholic acid. Background technique [0002] Hyodesoxycholic acid (Hyodesoxycholic Acid, HDCA) is a biochemical substance widely present in animal bile, with a content of 0.1% to 0.2%. Its chemical name is 3α, 6α-dihydroxy-5β-cholanic acid, and its molecular formula is C 24 h 40 o 4 , with a molecular weight of 392.58, easily soluble in ethanol, slightly soluble in acetone, very slightly soluble in ethyl acetate, chloroform or ether, almost insoluble in water. HDCA has the effects of lowering blood fat, antispasmodic and expectorant, and is clinically used to treat hyperlipidemia, atherosclerosis, tracheitis, viral upper respiratory tract inflammation in children, and dyspepsia caused by liver and gallbladder diseases; , Bacillus diphtheriae, Staphylococcus aureus, etc. have a certain inhibitory effect; as an active ingredient in Qingkailing injection, it has a good effect on the tre...

AI Technical Summary

Problems solved by technology

[0005] 1. Ethyl acetate or acetone recrystallization method. The main disadvantage of this technology is that although it can produce products with a melting point above 195, the liquid phase purity of the product is low, and the liquid phase purity of hyodeoxycholic acid is between 88-95%.

[0006] 2. Methyl esterification acetylate derivation method, although this technology can produce high-purity hyodeoxycholic acid, the purity of hyodeoxycholic acid is more than 98%, but strong carcinogens such as benzene are used in the process, and the process is cumbersome and unsuitable Industrial production

[0007] 3. Chromatographic column method. This technology first methylates the crude product of hyodecholate, and then separates it on a silica gel column. The main disadvantage of this method is that the production cycle is long and the production efficiency is low

[0008] Therefore, in order to improve the purity of hyodeoxycholic acid products and overcome the defects of existing HDCA purification methods such as complicated process, difficult operation, long production cycle, and high cost, it is urgent to develop a method that is easy to process large-scale production, low cost, and short production cycle. technical method