The present work deals with the development and validated simple HPLC/UV/FLD analytical procedure which enable the measurement of some of the most consumed pharmaceuticals in Jordan (Caffeine, Methotrexate, Diclofenac, Glimepiride, Ibuprofen) at concentration level of g/L. Separation was on RP-C8 column with 1 ml/min flow rate of 1:1 H2O, acetonitrile with 0.1% trifluoroacetic acid, extraction on C18 cartridges of 200 ml sample volume. Correlation coefficients of the pharmaceuticals calibration were higher than 0.997 using UV detector and 0.996 using FLD detector. Recoveries were ranged...