•Mg-Zn ferrites prepared by autocombustion, co-precipitation, spray pyrolysis.•Influence of structural features on magnetic properties of ferrites is determined.•The highest magnetization is achieved for Mg0.5Zn0.5Fe2O4 nanoparticles. Structural characteristics and magnetic properties of MgxZn1–xFe2O4 (x = 0.25; 0.5; 0.7) nanomaterials prepared by autocombustion, co-precipitation and spray pyrolysis methods were studied. Different characterization techniques are used to study the structural formation of the generated nanoparticles, namely X-ray diffraction (XRD), scanning (SEM) and transmission electron microscopy (TEM), infrared spectroscopy (FT-IR) and vibrating sample magnetometery (VSM). In case of citrate autocombustion and co-precipitation methods, the magnetization goes through a maximum at Mg0.5Zn0.5Fe2O4 composition, while the dependence on the composition is subtle for spray pyrolysis. An increase in temperature and duration of heat treatment during the synthesis process leads to a particle size growth and to a cation redistribution between spinel sub-lattices. These resulted in a significant increase in the specific magnetization of the particles generated by citrate autocombustion method. The nanoparticles synthesized by co-precipitation method exhibit superparamagnetic behavior with no coercivity at room temperature. Nonetheless, the materials prepared by spray pyrolysis and citrate autocombustion methods are found to possess small coercivity of 30–80 Oe. The highest specific magnetization at room temperature is referring to Mg0.5Zn0.5Fe2O4 nanoparticles obtained by citrate autocombustion method (30 emu/g). The revealed correlations can be used to synthesize spinel ferrite nanoparticles with well-defined collective properties for a wide spectrum of applications.