In this work, CeBTC (a cerium(III) 1,3,5-benzene-tricarboxylate), was used as a precursor for obtaining CeO2 nanoparticles (nanoceria) with better sensor performances than CeO2 nanoparticles synthesized by the solvothermal method. Metal–organic framework-derived nanoceria (MOFdNC) were functionalized with spheric gold nanoparticles (AuNPs) to further improve non-enzymatic electrode material for highly sensitive detection of prominent biocompound uric acid (UA) at this modified carbon paste electrode (MOFdNC/AuNPs&CPE). X-ray powder diffraction (XRPD) and transmission electron microscopy (TEM) analysis were used for morphological structure characterization of the obtained nanostructures. Cyclic voltammetry and electrochemical impedance spectroscopy, both in an [Fe(CN)6]3−/4− redox system and uric acid standard solutions, were used for the characterization of material electrocatalytic performances, the selection of optimal electrode modifier, and the estimation of nature and kinetic parameters of the electrode process. Square-wave voltammetry (SWV) was chosen, and the optimal parameters of technique and experimental conditions were established for determining uric acid over MOFdNC/AuNPs&CPE. Together with the development of the sensor, the detection procedure was optimized with the following analytical parameters: linear operating ranges of 0.05 to 1 µM and 1 to 50 µM and a detection limit of 0.011 µM, with outstanding repeatability, reproducibility, and stability of the sensor surface. Anti-interference experiments yielded a stable and nearly unchanged current response with negligible or no change in peak potential. After minor sample pretreatment, the proposed electrode was successfully applied for the quantification of UA in milk.