The electrochemical behaviors of diethylstilbestrol (DES) at a glassy carbon electrode were investigated by cyclic voltammetry, linear sweep voltammetry, and differential pulse voltammetry (DPV). Based on these, a sensitive and selective DPV method was developed for determination of DES. The linear response range of DES is 1.0 x 10(-4)-2.0 x 10(-6) mol/L and the detection limit was 8.0 x 10(-8) mol/L. The developed method has been used for the pharmacokinetics of DES in rabbit blood plasma.