Analytical chemistry plays a fundamental role in proposing fast and reliable procedures to analyze food samples. Proper selection and introduction of complementary foods during the breastfeeding period and childhood reduce the vulnerability to micronutrient deficiencies. This study aimed to propose a sensitive approach for the promotion of adequate food supplements regarding Cd, Fe, Pb, and Zn content. These metals were determined using flame atomic absorption spectrometry (Fe and Zn) and thermospray flame furnace atomic absorption spectrometry (Cd and Pb). A simple procedure mixing the sample (100 mg) with 0.1 mol/L HCl was proposed. Cadmium and Zn showed suitable results when a bovine liver certified sample (SRM 1577b) was studied, and the Fe content was strongly correlated to the size of the particle. Cadmium and Pb were not found in the food samples studied.