This study investigates the synthesis of nanostructured magnesium oxide (MgO) using the auto-combustion method with urea (MgO-U), glycine (MgO-G), and citric acid (MgO-C) as fuels, followed by subsequent calcination. The selection of fuel plays a crucial role in determining the morphology of the nanostructures.X-ray diffraction (XRD) analysis confirms that the samples exhibit a well-crystallized structure with the desired phase and are free of impurities. Field emission scanning electron microscopy (FESEM) shows that MgO-U nanoparticles have diameters ranging from 10 to 20nm, MgO-C nanoparticles from 60 to 80nm, and MgO-G nanoparticles from 80 to 100nm. These MgO nanomaterials are specifically engineered for adsorption applications, aimed at removing toxic organic dyes and fluoride ions from aqueous solutions. Results demonstrate that MgO-G nanoparticles exhibit superior adsorption activity compared to MgO-U and MgO-C nanoparticles, with maximum uptake capacities of 1429 and 14mg/g, respectively. The adsorption processes adhere to second-order kinetic model. These findings highlight the potential application of the synthesized MgO nanoparticles for mitigating water pollution by adsorbing pollutants from aqueous media.