This study focused on composites of magnetite magnetic nanoparticles (MNP) and poly(lactic acid) (PLA) prepared via sonochemical synthesis. The evaluation of MNP loadings (2, 5, 10, 15, and 20 wt.%) provided insights into the structural and reactivity properties of the materials. Methods used included XRD, FT-IR and Raman spectroscopy, SEM and TEM microscopy, textural and thermal analysis (TG and DTA), and magnetic property measurements. The agreement between theoretical and experimental MNP loadings was good. XRD patterns showed predominantly MNP and semicrystalline phases, with a minor maghemite phase detected by FT-Raman and magnetic measurements. FT-IR analysis revealed interactions between MNP and PLA, confirmed by thermal analysis showing higher transition temperatures for the composites (145 °C) compared to pure PLA (139 °C). FT-Raman spectra also indicated that PLA helps prevent iron oxide oxidation, enhancing nanoparticle stability. SEM and TEM micrographs showed well-dispersed, spherical nanoparticles with minimal agglomeration, dependent on MNP loading. The nanocomposites exhibited low N adsorption, resulting in low surface area (2.1 m/g) and porosity (0.03 cm/g). Magnetic analysis indicated that in the 2MNP/PLA sample, MNP were in a superparamagnetic-like regime at 300 K, suggesting good dispersion of 2 wt.% MNP in the PLA matrix.