A method for the preparation and purification of chenodeoxycholic acid from a poultry and animal bile or a waste waste of bilirubin hyodeoxycholic acid. The process is saponification, oxidation decolorization, clarification treatment, preparation of a calcium salt, secondary calcium salt, macroporous adsorption resin adsorption, analytical crystallization, refining and other production processes. The whole process is environmentally friendly, safe non-toxic, low cost, easy to industrial scale production chenodeoxycholic acid. Content of 98% or more, high performance liquid chromatography. Other substances: hyodeoxycholic acid content <0.5%, lithocholic acid <0.1%. Thin layer chromatography: a chenodeoxycholic acid main spot, a slight hyodeoxycholic acid spot.
A method for the preparation of chenodeoxycholic acid, characterized in that the raw material used is animal bile, bile cream or its extraction of bilirubin, hyodeoxycholic acid after the following, including the following steps: (1) Saponification.10% -15% NaOH , The temperature is 100-120 ℃, time 18-26 hours; (2) Oxidation, industrial hydrogen peroxide 0.5-2%, in order to achieve white-like; (3) Clarification, with 1 + 1 natural clarifier 0.5-, the temperature is 80-100 ℃, pH 9-14, 0.5-2 hours, plate and frame filter to clarify the filtrate; (4) With dilute hydrochloric acid pH2-3, obtained cholic acid, ethyl acetate 8 times dissolved, activated carbon 1 and refluxed for 2 hours. The filtrate was concentrated to 1/5 crystallization to obtain hyodeoxycholic acid, which was recrystallized from ethyl acetate to obtain a hyodeoxycholic acid having a melting point of 198 °C or higher. (5) The ethyl acetate of the secondary hyodeoxycholic acid was recovered and left. (6) A calcium salt: add dark brown bile paste 1 times the amount of industrial calcium chloride, the content of the calcium salt, high performance liquid chromatography detection requirements; molar ratio chenodeoxycholic acid: calcium chloride = 1: 1, 60-80 ℃, 2 hours, plate and frame filter after adding sodium carbonate replacement chenodeoxycholic acid, adding the molar ratio of calcium chloride. (7) Secondary calcium salt to the ratio of (6), the process conditions into calcium salt, with 300-1000 times the deionized water washing, Bi, the temperature of 90-100 ℃. (8) Crude chenodeoxycholic acid dissolved in alkaline water pH 6.0-8.0 weak alkaline or strong alkaline macroporous resin adsorption, saturation, washed to remove impurities, dilute alkali solution. (9) Dissolve chenodeoxycholic acid in acetonitrile mixed solvent for 2 hours, add 10% of activated carbon, heat filtration, crystallization; recrystallization to be obtained by thin layer chromatography to determine the starting point of the reception, the end point, pH3 vacuum drying; chenodeoxycholic acid boutique, content greater than or equal to 98% HPLC, containing hyodeoxycholic acid <0.5% HPLC, lithocholic acid <0.1%, thin layer chromatography TLC: one chenodeoxycholic acid main spot, one slight hyodeoxycholic acid spot.