This work described a sensitive method for determination of metoprolol in rabbit plasma. The method involved purification by ultrafiltration, derivatization with Fluorescein isothiocyanate, separation by capillary electrophoresis and determination by laser induced fluorescence detector. Other components in plasma including a variety of amino acids and proteins did not interfere with the determination of metoprolol under experimental conditions. The assay had a wide range (2.0-500 ng/mL) of linearity and a detection limit of 0.8 ng/mL. The intra and inter day precisions of the QC samples were satisfactory with RSD less than 10% and accuracy within 10%. This method was successfully applied to pharmacokinetic study of meto prolol in rabbit blood.