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A copper oxide/cerium oxide nanocomposite (CuO/CeO2, NC) was synthesized via a novel method using a metal–organic framework as a precursor. This nanomaterial was characterized by Fourier transform infrared spectroscopy (FTIR), powder X-ray diffraction (PXRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), dynamic light scattering size analysis (DLS), and zeta potential. The PXRD showed the successful synthesis of the CuO/CeO2 NC, in which the 2theta values of 35.55° (d = 2.52 Å, 100%) and 38.73° (d = 2.32 Å, 96%) revealed the existence of copper (II) oxide. FTIR analysis showed the CeO2, hydroxyl groups, absorbed water, and some residual peaks. The solid phase analysis by FESEM and TEM images showed mean particle sizes of 49.18 ± 24.50 nm and 30.58 ± 26.40 nm, respectively, which were comparable with crystallite size (38.4 nm) obtained from PXRD, but it appears the CuO/CeO2 NC was not evenly distributed and in some areas, showed it was highly agglomerated. The hydrodynamic size (750.5 nm) also showed the agglomeration of the CuO/CeO2 NCs in the solution, which had a negatively charged surface. The CuO/CeO2 NCs showed anti-proliferative activity against human breast cancer cell line (MCF-7) in a dose- and time-dependence way, while affecting normal cells less significantly. [ABSTRACT FROM AUTHOR]