Determination of fluocortolone pivalate and fluocortolone hexanoate in suppositories using reverse-phase HPLC.

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.

False-positive results in the radioimmunoassay detection of stilbene derivatives after administration of fluorinated corticosteroids to animals.

During routine inspections, indications were found that the therapeutic use of fluocortolone or dexamethasone can cause false-positive results in the detection of stilbene derivatives by radioimmunoassay (RIA) in samples of animal origin. After experimental application of the fluorinated corticosteroids to rabbits or calves, the assumed false-positive RIA results were confirmed. The kinetics after application of dexamethasone were concomitant with the elimination of radioactive [3H]dexamethasone. Furthermore, it could be demonstrated that [3H]dexamethasone was transformed in the faeces of rabbits and calves. The metabolites formed were not completely separated by the extraction procedure used for the RIA and seemed to be responsible for the false-positive results.