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The development of a pH‐responsive, biocompatible polymeric carrier for controlled delivery of bioactive agents holds significant practical value for pharmaceutical applications. In this study, we used the gelation method to make pH‐responsive polymeric microbeads using sodium alginate (SA), poly(vinylpyrrolidone‐co‐vinyl acetate) (PVPVA), and nickel zinc ferrite (NZF) nanoparticles for controlled release of doxorubicin (DOX). The generated microbeads are characterized using various techniques, including Fourier‐transform infrared spectroscopy, X‐ray diffraction, scanning electron microscopy, and transmission electron microscopy. Swelling studies reveal enhanced permeability at pH 6.4, and in vitro release studies demonstrate a higher release rate at pH 6.4 compared to pH 2.0. Cytotoxicity tests on MCF‐7 cells (a type of breast cancer cell line) showed that NZF‐loaded microbeads, especially SP‐NZFNPs‐DOX, were more effective than other carriers, indicating their potential usefulness in cancer treatment. Furthermore, biocompatibility tests demonstrate that the SA/PVPVA microbeads and nanoparticles are biocompatible with 3T3 fibroblasts. This study contributes valuable insights to the evolving landscape of nanotechnology in cancer treatment, emphasizing the synergistic role of NZF nanoparticles, SA, and PVPVA in optimizing drug delivery systems. [ABSTRACT FROM AUTHOR]