Anodic stripping voltammetry is useful instrumental method for trace element determination in biological materials. It is however extremely demanding to the quality of the sample preparation process. The high-pressure microwave assisted digestion seems to meet its requirements. The differential pulse anodic stripping voltammetry technique was used for determination of cadmium, copper, lead and zinc in certified reference materials both of plant and of animal origin to prove the analytical properties of such sample preparation method. The found concentrations have been in satisfactory agreement with the certified values. The elaborated digestion procedure is greatly universal and has required accuracy and precision.