Recently Ni−Co mixed oxide nanoparticles have received tremendous attention for their application potential in electrochemical devices, biosensing, and biomedical treatments. However, the biomedical application of these nanostructures is severely restricted due to their poor magnetic properties. Here we present the fabrication of nickel cobaltite nanoparticles of 17−40 nm size range with different Ni contents by a simple glycolmediated sol−gel process. We demonstrate that, by controlling Ni content in the mixed oxide nanoparticles, their lattice structure can be transformed from inverse spinel to partially inverse spinel lattice. Moreover, by controlling the site occupancy of Co 2+,3+ and Ni 2+,3+ ions, their net magnetization can be enhanced substantially. The nanoparticles prepared with a nickel/cobalt ratio of 0.25 manifest superparamagnetic behavior with room temperature saturation magnetization as high as 66.3 emu/g (2.75 μ B ) and coercivity as low as 85 Oe, which indicate their great potential for biomedical applications such as hyperthermia and targeted drug delivery.