<p>The combustion method was used to create the calcium copper oxide nanoparticles <b>(</b>CaCuO₂Nps). The morphology and characterization of the structure were investigated through the use of powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron spectroscopy (SEM), and energy dispersive X-ray analysis (EDAX). Electrochemical response of uric acid (UA) and tyrosine (TY) atcalcium copper oxide nanoparticles modified glassy carbon electrode <b>(</b>CaCuO₂ Nps/MGCE) was studied using electrochemical impedance spectroscopy <b>(</b>EIS), cyclic voltammetry (CV), and differential pulse voltammetry (DPV) techniques.CaCuO₂ Nps/MGCE proved stability and a powerful promoting effect for UA and TY detection. The scan rate studies demonstrated the electrode method was diffusion-controlled. The concentration studies revealed the lower LOD and LOQ. The pH studies indicate that UA and TY were electrochemically oxidized with an equivalent number of protons and electrons. The detection of both UA and TY, the CaCuO₂Nps/MGCE demonstrated outstanding electrocatalytic activity. Simultaneous measurements confirmed that the peak-to-peak potential variance between UA and TY was enough for their individual as well as simultaneous determination.Further evidence of the fabricated electrochemical sensor’s useful applicability was obtained through repeatability, reproducibility, stability, and real sample analysis tests. The reproducibility study yielded relative standard deviation (RSD) values of 0.86% for 25 × 10^–4 M UA and 0.84% for 25 × 10^–4 M TY (<i>n</i> = 5), along with excellent recovery in real sample analyses.</p>