The electrochemical behavior of ascorbic acid (AA), dopamine (DA), and uric acid (UA) on a DL-norvaline-modified glassy carbon electrode (GCE) was studied by cyclic voltammetry. The bare GCE failed to distinguish the oxidation peaks of AA, DA, and UA in phosphate-buffered solution (pH 5.0), while the DL-norvaline-modified GCE could separate them efficiently. In differential pulse voltammetric (DPV) measurements, the modified electrode resolved the overlapped voltammetric responses of AA, DA, and UA into three well-defined voltammetric peaks. Under optimum conditions, the anodic peak currents of DPV for AA, DA, and UA were proportional to the concentration in the range of 20-400, 1-40, and 15-180 mu mol/L, respectively, with a correlation coefficient (r) of around 0.998. The detection limits were 5, 0.3, and 10 mu mol/L (S/N = 3) for AA, DA, and UA, respectively. Satisfactory results were achieved for the determination of AA in vitamin C tablets, DA in a dopamine ampoule sample, and UA in human blood serum samples.