Process for the recovery of a transition metal from an aqueous solution containing a complex of the transition metal with a cyclic phosphite by hydrolyzing the cyclic phosphite, contacting the hydrolysis reaction mixture with a compound forming a water-stable complex with the transition metal, extracting the reaction mixture thus formed with an organic extraction agent for the water-stable complex and separating an organic extract phase containing the transition metal from an aqueous raffinate phase. The process is particularly suitable for the recovery of the Rh or Co from spent hydroformylation catalysts and of Pd from spent carbonylation catalysts.