The present work describes the development of a microwave-assisted extraction procedure for the determination of zinc and copper in cereal samples employing flame atomic absorption spectrometry (FAAS). A Doehlert design was carried out in order to determine the optimum conditions for the procedure through response surface study. Three variables (irradiation power, time, and temperature) were regarded as factors in the optimization study. The working conditions were established as a compromise between optimum values found for each analyte. These values were 110.0 °C, 176.0 W, and 16.0 min, for temperature, irradiation power, and time, respectively. The accuracy of the optimized procedure was evaluated by analysis of certified reference materials. The procedure proposed was applied for the determination of copper and zinc in cereal samples.