Magnetic nanoparticles (MNPs) that exhibit high specific loss power (SLP) at lower metal content are highly desirable for hyperthermia applications. The conventional co-precipitation process has been widely employed for the synthesis of magnetic nanoparticles. However, their hyperthermia performance is often insufficient, which is considered as the main challenge to the development of practicable cancer treatments. In particular, ferrite MNPs have unique properties, such as a strong magnetocrystalline anisotropy, high coercivity, and moderate saturation magnetization, however their hyperthermia performance needs to be further improved. In this study, cobalt ferrite (CoFe2O4) and zinc cobalt ferrite nanoparticles (ZnCoFe2O4) were prepared to achieve high SLP values by modifying the conventional co-precipitation method. Our modified method, which allows for precursor material compositions (molar ratio of Fe+3:Fe+2:Co+2/Zn+2 of 3:2:1), is a simple, environmentally friendly, and low temperature process carried out in air at a maximum temperature of 60 °C, without the need for oxidizing or coating agents. The particles produced were characterized using multiple techniques, such as X-ray diffraction (XRD), dynamic light scattering (DLS), transmission electron microscopy (TEM), ultraviolet-visible spectroscopy (UV–Vis spectroscopy), and a vibrating sample magnetometer (VSM). SLP values of the prepared nanoparticles were carefully evaluated as a function of time, magnetic field strength (30, 40, and 50 kA m−1), and the viscosity of the medium (water and glycerol), and compared to commercial magnetic nanoparticle materials under the same conditions. The cytotoxicity of the prepared nanoparticles by in vitro culture with NIH-3T3 fibroblasts exhibited good cytocompatibility up to 0.5 mg/mL. The safety limit of magnetic field parameters for SLP was tested. It did not exceed the 5 × 109 Am−1 s−1 threshold. A saturation temperature of 45 °C could be achieved. These nanoparticles, with minimal metal content, can ideally be used for in vivo hyperthermia applications, such as cancer treatments.