Abstract Nowadays, multifunctional nanocarriers have attracted significant attention due to their potential to improve therapeutic efficacy while reducing toxicity. In this study, microbeads loaded with doxorubicin (DOX), a widely used chemotherapeutic agent in cancer treatment were synthesized via precipitation polymerization. To achieve this, various nanomaterials, including graphene oxide (GO), Fe 3 O 4 , Fe 3 O 4 @GO (FGO), Fe 3 O 4 @GO@DOX (FGOD), and microbeads (mFGOD), were prepared. Structural, chemical, and thermal properties were analyzed using various characterization techniques. Additionally, morphological and elemental characterization was conducted via scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy‐dispersive X‐ray spectroscopy (EDX). The microbeads exhibited smooth surfaces and heterogeneous size distribution. The drug loading and release capacities of the obtained microspheres were quantitatively determined using analytical techniques at pH 6 and 7.4, and release kinetics were analyzed using various kinetic models. The drug loading efficiency was 80%, and the microbeads showed pH‐responsive release with higher drug release at pH 6 than at pH 7.4. Biological evaluations demonstrated a significant reduction in relative cell viability in the YKG1 glioblastoma cell line after 24 and 48 h, whereas no substantial cytotoxic effects were observed in healthy HUVEC endothelial cells, even after 48 h. Their cytocompatibility highlights their potential as a versatile biomedical platform.