AbstractMagnetic hyperthermia therapy (MHT) is a highly promising therapeutic modality for the treatment of different kinds of cancers and malignant tumors. The therapy is based on the concept that; iron oxide nanoparticles deposited at cancer sites can generate heat when exposed to an alternating current magnetic field or near infrared radiation and consequently destroying only the cancer cells by exploiting their vulnerability to heat. The fact that the treatment is at molecular level and that iron oxide nanoparticles provide more guided focus heating justifies its efficacy over treatment such as surgery, radiation therapy and chemotherapy. Nevertheless, the spread of MHT as the next-generation therapeutics has been shadowed by insufficient heating especially at the in vivo stage. This can be averted by modifying the iron oxide nanoparticle structure. To this end, various attempts have been made by developing a magnetic hybrid nanostructure capable of generating efficient heat. However, the synthesis method for each component (of the magnetic hybrid nanostructure) and the grafting process is now an issue. This has a direct effect on the performance of the magnetic hybrid nanostructure in MHT and other applications. The main objective of this review is to detail out the different materials, methods and characterization techniques that have been used so far in developing magnetic hybrid nanostructure. In view of this, we conducted a comprehensive review and present a road map for developing a magnetic hybrid nanostructure that is capable of generating optimum heat during MHT. We further summarize the various characterization techniques and necessary parameters to study in validating the efficiency of the magnetic hybrid nanostructure. Hopefully, this contribution will serve as a guide to researchers that are willing to evaluate the properties of their magnetic hybrid nanostructure.