6-Mercapto purinylazo resin has been used as solid phase extractor. Based on solid phase extraction, the present work describes the preconcentration and determination of copper, zinc and cadmium in certified biological samples after microwave-assisted digestion. The exchange capacity of the resin, the sorption and desorption of metal ions, and the effect of diverse ions have also been determined. The results show that the resin is highly selective for determination of these biologically significant metals. The method is simple, rapid and free from interferences and can be used routinely.