A new spectrophotometric method has been developed for the rapid, accurate and inexpensive determination of xylometazoline (XMH) in its pure form and in some pharmaceutical preparations, using the first derivative technique. It was found that this technique enables us to quantitatively estimate xylometazoline in a range of concentrations (5-50 µg.ml-1), the height of the peak above the base line of the wavelengths (268 and 292 nm) was taken advantage of. The obtained results showed that the method is accurate and has good agreement, as the percentage recovery was (95-100%), while the RSD value was (0.030-0.300%) for wavelengths respectively, the method was applied to a number of commercial pharmaceuticals successfully.