Application of capillary zone electrophoresis with electrochemical detection to the identification and quantitative determination of uric acid in human urine as well as plasma is described. This work was carried out in a 30 cm x 25 microm I.D. fused-silica capillary with tricine buffer and a carbon fiber bundle was employed as a working electrode, the working voltage in amperometric detection was set at +0.80 V (vs. SCE). The sample constituent is identified by stopped flow-linear sweep voltammetry. Under optimal conditions, a lower detection limit of 0.48 fmol was obtained for uric acid.