A glassy carbon electrode modified with LaHCF was constructed and was characterized by cyclic voltammetry (CV) and electrochemical impedance spectrum (EIS). The resulting LaHCF modified glassy carbon electrode had a good catalytic character on uric acid (UA) and was used to detect uric acid and ascorbic acid (AA) simultaneously. This modified electrode exhibits potent and persistent electron-mediating behavior followed by well-separated oxidation peaks towards UA and AA with activation overpotential. For UA and AA in mixture, one can well separate from the other with a potential large enough to allow the determination of one in presence of the other. The DPV peak currents obtained increased linearly on the UA in the range of 2.0×10−7 to 1.0×10−4 mol/L with the detection limit (signal-to-noise ratio was 3) for UA 1.0×10−7 mol/L. The proposed method showed excellent selectivity and stability, and the determination of UA and AA simultaneously in urine was satisfactory.