New non-mechanical process of micronization, capable to reduce the particle size of digoxin from ordinary level to a selected micrometer range. Micronization is obtained via a specific treatment, to be performed on a purified and concentrated digoxin solution in an organic solvent. The purified and concentrated digoxin solution is obtainable via a sequence of solvent treatments； then, after reaching the required concentration, the solution is further concentrated, obtaining the precipitation of digoxin； the reaction mixture is then added with methanol under stirring for a suitable time. The recovered precipitate consists in a digoxin with particle size comprised between 20 and 30 micrometers (for at least 90% by weight of the obtained particles), and exempt from degradation products.
