A high performance liquid chromatographic procedure is presented for the simultaneous determination of naphazoline nitrate and antazoline sulphate in pharmaceutical combinations. An aliquot of the sample is dissolved in water containing N-butyryl-4-aminophenol as an internal standard and is chromatographed on a supelcosil LC-8 (5 μm) (150 mm × 4.6 mm i.d.) column using a mobile phase of acetonitrile/water/triethylamine (40:59.75:0.25) adjusted to pH 4.5 by glacial acetic acid. This proposed HPLC methodology has the advantages of being fast and stability-indicating.