Fluocortolone and its esters are synthetic corticosteroids used topically in the treatment of various skin disorders. A method that can be successfully used for the separation and determination of fluocortolone pivalate and fluocortolone hexanoate in suppositories was developed. This method is based on reverse-phase HPLC on Supelcosil LC-18 (25 cm x 4.6 mm, 5 microns), using methanol-acetonitrile-water-glacial acetic acid (17:46:37:0.4 v/v/v/v) as mobile phase at a flow rate of 3.0 ml/min. Detection was carried out using a UV detector at 238 nm. The method developed was validated, and calibration curves were established dependent on peak area. The validated ranges for fluocortolone pivalate and fluocortolone hexanoate are 15-305 micrograms/ml (r = 0.9995) and 15-315 micrograms/ml (r = 0.9996), respectively. The limits of detection and the limits of quantification for both esters were also determined.