The Zinc-doped cerium oxide nanocomposite (ZnO/CeO₂ NC) was synthesized using a metal-organic framework as a precursor through the combustion method. It was characterized by powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR), field emission electron microscopy (FESEM), energy dispersive analysis (EDX), transmission electron microscopy (TEM), dynamic light scattering (DLS), and ξ-potential. The PXRD demonstrated the successful synthesis of ZnO/CeO₂ NC with a crystallite size of 31.9 nm. FESEM and TEM images displayed hexagonal and spherical morphologies, and the solid-phase size was 65.03 ± 30.86 nm for ZnO/CeO₂ NCs. DLS, TEM, and FESEM showed that the NCs have a high tendency for agglomeration/aggregation in both aqueous media and solid phase. The anticancer attributes of ZnO/CeO₂ NC were investigated against Liver cancer cells (HepG2), which showed inhibition of cancer cell growth on a concentration-dependent gradient. The cell toxicity effects of ZnO/CeO₂ nanocomposites were also studied toward NIH-3T3, in which the data displayed the lower toxicity of NC compared to the HepG2 cell line.