METHOD FOR PREPARING HIGH-CONTENT BILIRUBIN IX α USING BILIVERDIN IX α

摘要

The present invention relates to the field of bilirubin IX α preparation. Disclosed is a method for preparing high-content bilirubin IX α using biliverdin IX α. The method comprises the following steps (a hydrolysis-before-reduction route): dropping a methanol solution of sodium hydroxide to an alcohol solution of biliverdin IX α diester, adding water to the mixture for hydrolysis, adjusting the pH of the mixture to a range from 4 to 5 using a weak acid, carrying out rotary evaporation to remove a solvent, carrying out washing to remove an organic slat, and carrying out vacuum drying to obtain biliverdin IX α; andadding a radical scavenger (a stabilizer) to an alcohol solution of biliverdin IX α, adding a reducing agent, i.e., borohydride, to the mixture, instantly adding ketone to decompose the excess reducing agent when the reduction reaction ends, then adjusting the pH of the mixture to a range from 4 to 5 using a weak acid, carrying out rotary evaporation to remove a solvent, carrying out washing, and carrying out methanol-chloroform refining to obtain bilirubin IX α having a content greater than 97%. The method does not require chromatographic separation, features moderate reaction conditions, low costs, and convenient operations, and is suitable for large-scale industrial production.