A mixture of three distinct cerium precursors (Ce(NO 3 ) 3 •6H 2 O, CeCl 3 •7H 2 O, and Ce(CH 3 COO) 3 •H 2 O) was used to prepare cerium oxide nanoparticles (CeO 2 NPs) in a polyol-mediated synthesis. Different ratios of diethylene glycol (DEG) and H 2 O were utilized in the synthesis. The properties of the synthesized CeO 2 NPs, such as structural and morphological properties, were investigated to observe the effect of the mixed cerium precursors. Crystallite sizes of 7−8 nm were obtained for all samples, and all synthesized samples were confirmed to be in the cubic phase. The average particle sizes of the spherical CeO 2 were between 9 and 13 nm. The successful synthesis of CeO 2 can also be confirmed via the vibrational band of Ce−O from the FTIR. Antidiabetic properties of the synthesized CeO 2 NPs were investigated using α-glucosidase enzyme inhibition assay, and the concentration of the synthesized CeO 2 NPs was varied in the study. The biocompatibility properties of the synthesized CeO 2 NPs were investigated via cytotoxicity tests, and it was found that all synthesized materials showed no cytotoxic properties at lower concentrations (62.5−125 μg/mL).