Determination of aminoglutethimide enantiomers as a dansyl derivative in plasma by HPLC has been achieved using cellulose tris(3,5-dimethylphenyl carbamate) chiral stationary phase known as Chiralcel OD, and a mobile phase consisted of ethanol-cyclohexane-methanol (95:5:2 nu/nu/nu). The limit of detection for each enantiomer of aminoglutethimide using fluorescence detector was 20 ng ml(-1)