Magnetic
nanoparticles (MNPs) are one of the most promising candidates
for their use as theranostic agents in the biomedical field due to
their potential as contrast agents in magnetic resonance imaging (MRI)
and also as heat generators in magnetic hyperthermia treatments. However,
despite the large number of publications about this topic, just some
few systematic studies about the influence of MNPs composition on
their theranostic capabilities have been carried out. In this work,
we show a detailed methodology for the preparation of highly monodisperse
iron oxide-based MNPs with different cobalt, zinc, and manganese doping
extents in the superparamagnetic regime. We aim to provide the tools
to control the composition of the particles, as well as for their
functionalization to make them highly stable in biological-mimicking
media. Procedures to measure the capability of the particles as magnetothermal
and MRI negative contrast agents as well as to analyze the influence
of doping on such properties are also reported. In all experiments,
the applied alternating magnetic fields were within the maximum allowed
amplitude, frequency, and amplitude·frequency product range for
potential validation of the experimental data toward the potential
translation of the present MNPs to the clinical practice.