A flow injection analysis (FIA) of doxazosin mesylate (DOX) using UV detection is described in this study. The best solvent system was found to be consisting of 0.1 mol l(-1) acetate buffer at pH 4 having 10%MeOH. A flow rate of 1 ml min(-1) was pumped and active material was detected at 365 nm. The calibration equation was linear in the range of 1.3 x 10(-5) to 6.4 x 10(-5) mol l(-1). Limit of detection and limit of quantitation were calculated to be 1.6 x 10(-6) and 4 x 10(-6) mol l(-1) with a RSD 1.27 and 1.16% (n = 8), respectively. The proposed method was applied to the determination of DOX in the pharmaceutical preparations. The results were compared with those obtained from UV-Spectrophotometry. The results showed that there is a good agreement between FIA method and UV-Spectrophotometry. The validation studies were realised by the related applications and the results were evaluated statistically. According to the results, insignificant difference was observed between the methods. (C) 2001 Published by Elsevier Science B.V.