The increasing use of engineered nanomaterials in commercial manufacturing and consumer products presents an important toxicological concern. Superparamagnetic zinc-cobalt ferrite nanoparticles (SFN) emerge as a promising tool for early cancer diagnostics and targeted therapy. However, toxicity and biological activities of SFN should be evaluated in vitro and in vivo in animal before any clinical application. In this study we aim to synthesize and characterize such objects using polyol process in order to assess its nanotoxicological profile in vitro as well as in vivo. The produced particles consist of a cobalt-zinc ferrite phase corresponding to the Zn 0.8 Co 0.2 Fe 2 O 4 composition. They are isotropic in shape single crystals of 8 nm in size. The thermal variation of their dc-magnetization confirms their superparamagnetic behavior. In vitro, acute exposure (4 h) to them (100 g mL −1) induced an important decrease of healthy Human Umbilical Vein Endothelial Cells (HUVECs) viability. In vivo investigation in New-Zealand rabbits revealed that they lead to tissue toxicities; in lungs, liver and kidneys. Our investigations report, for the first time as far as we know, that SFN exhibit harmful properties in human cells and mammals.