Objective. Spectrophotometry is one of the most widely used methods in the pharmaceutical analysis, both for the identification and for the assay of drugs. The main advantages of the method are the relative simplicity of the experiment, high sensitivity, specificity and efficiency. Therefore, the objective of the present work was development of spectrophotometric method for the assay of xylometazoline.Materials and methods. Xylometazoline working standard, alizarin red, ethanol and the sample of finished dosage form were used. Absorption of the reaction products was measured using spectrophotometr Specord 200.Results. The optimal conditions for the quantitative determination of xylometazoline in the content of pharmaceutical drugs were established. It was experimentally established that xylometazoline reacts with alizarin red to formation the colored reaction product with absorption maximum at 526 nm. The proposed method was subjected to validation tests according to the requirements of the State Pharmacopoeia of Ukraine. The method was validated for the parameters like linearity, precision, accuracy, robustness and scope of application. Beer’s law was obeyed over the concentration range of 2,40-4,00 mg/100 ml with correlation coefficient 0,9978. Parameters of linear dependence were calculated with the help of regression analysis by means of least squares. The border of determination at optimum conditions was 1,89 μg/ml, that showed the high sensitivity of the reaction. Coefficients of stoichiometric relationship were also determined by means of molar ratios and continuous changes. The proposed method meets the requirements of the State Pharmacopoeia of Ukraine, which are advanced to the methods for the assay of pharmaceutical formulations.Conclusion. A highly sensitive, economical, reproducible spectrophotometric method for the assay of xylometazoline has been developed and validated. This procedure is successfully applied for dosage form analysis. Investigation results show that the procedure is highly sensitive, precise, simple in performance and relevant to be applied at the quality control laboratories for dosage forms.