A process for preparing dermatan sulphate (DS) of pharmaceutical purity from animal organs rich in micropolysaccharides (MPS), by: a) stabilizing the fresh organs by freezing them either as such or in the form of powder, b) micronizing the material containing the MPS with an aqueous CaCl.sub.2 solution, c) digesting the homogenate comprising the raw material and the CaCl.sub.2 with proteolytic enzyme at alkaline pH and at low temperature, d) acidifying, heating and filtering the lysate, e) treating the filtrate with quaternary ammonium salts able to undergo complexing with and thus precipitate either the DS alone or all the MPS selectively, f) recovering and purifying the DS either directly from the ammonium salt complex containing it or from the complex obtained from the mixture of ammonium salt complexes of all the MPS by fractional solubilization with acetone.