Nanotechnology has a wide and interesting scientific and industrial potential in technological applications. In general terms, nanoparticle (NP) synthesis demands high temperatures, long reaction time and, expensive/toxic precursors. The main goal of this work is to optimize and expand NP synthesis from a glycerol-urea (GU) route. The GU route utilizes glycerol as a basic solvent and allows the use of additives (such as urea and other derivatives) in order to control the size and shape of the NPs. So as to produce metal oxide NPs (ZnO, CuO, and Fe3O4), different reaction parameters were modified during synthesis. X-ray diffraction (XRD), X-ray fluorescence spectroscopy (XRF) and transmission/scanning electron microscopy (TEM/SEM) were utilized as means of NPs characterization. The GU route promoted fast ZnO NPs formation (<1 hour) with high purity, with average purity of 99.8%. The ZnO NPs maintained their expected average size of 15 to 25 nm, with up to 10:1 glycerol:urea molar ratio. Higher proportion than 10:1 showed NPs without uniform particle size. The ratio of Zn 2+ /-OH above 1:4 lead to micrometric ZnO particles. Synthesis utilizing glycerol-water or, only glycerol, resulted in micrometric ZnO particles. The substitution of urea for acetone, thetramethylurea, and formamide yielded ZnO NPs with high crystallinity and uniform spherical morphology. The dimethylurea or water substitution leads to non-uniform micrometric particles, revealing the structural influence of the organic additive in nucleation process of NPs formation. Experiments for CuO and Fe3O4 showed no formation of metal oxide NPs, but nitrates or thiol complexes resulting from the urea reaction with copper and iron. CuO NPs were obtained only after calcination in a muffle oven, resulting in single monoclinic structure and nanometric crystallite size.