Magnetic resonance imaging (MRI) is the technique for the visualization of targeted macromolecules or cells in biological system. Nowadays, superparamagnetic iron oxide nanoparticles (SPIONs) have been attracted and remarkably emerging as a negative contrast agent (T2-weighted) offering sufficient detection sensitivity as compared to positive contrast agent (T1-weighted). In the present chapter, we first introduce the necessary background of superparamagnetic iron oxide-based nanoparticles and MRI taking into an account to discuss both T1–T2-weighted imaging. The liquid-based synthesis methods of SPIONs and their applicability in MRI have been thoroughly revised. Finally, several nanohybrids such as magnetic-silica, magneto-luminescent, magneto-plasmonic along with ferrite-based SPIONs are thoroughly presented in light of MRI application.