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.