The aim of this work was to investigate a simple and reliable method for the determination of trace amounts of famotidine, fluconazoie and ketoconazole in bulk powder and in their pharmaceutical dosage forms. Also to study the different factors affecting the sensitivity of the synchronous technique in order to improve the measurement The sample was prepared in methanol in case of famotidine and ketoconazole, and in water, after dissolution in methanol, in case of fluconazoie. The fluorescence intensity was recorded at 384 (ex. at 284 nm), 285 (ex. at 255 nm) and 364 nm(ex. at 239 nm) for famotidine, fluconazole and ketoconazole respectively. The calibration curves were linear over the concentration ranges 15 50, 0. 20–10 and 0. 02–0. 4 μg/ml for famotidine, fluconazole and ketoconazole respectively.