Three Simple, accurate and reproducible UV spectrophotometric methods were established for the assay of pyrilamine maleate (PYRA) based on the formation of ion-association products between PYRA and cobaltous thiocyanate (CTC), citric acid (CA) and Alizarin red S (ARS). The optical characteristics such as Beers law limits, molar absorptivity and Sandell’s sensitivity for the methods (M1-M3) are given. The absorbance was measured at 620 (CTC-M1), 580 (CA-M2) and 420 nm (ARS M3). Regression analysis using the method of least squares was made to evaluate the slope (b), intercept (a) and correlation coefficient (r) and standard error of estimation (Se) for each system. Determination of Pyrilamine in bulk form and in pharmaceutical formulations was also incorporated.