Liquid adsorption chromatography, in combination with full adsorption -desorption and precipitation-redissolution techniques is a powerful procedure for the fractionation of mixtures in the synthesis of star polymers. An easy separation of 4- and 6 arm star poly(methyl methacrylates)s from their single arm precursors could be carried out by both procedures with differences of separation efficiency also dependent on the molecular weight of the precursor and the number of arms.