A stability-indicating analytical method is described for the simultaneous determination of nitrate, and if present, its reductive degradation product, nitrite, in toothpastes. Nitrate and nitrite were extracted from the toothpaste using distilled water and separated from other water-soluble excipients by two RP-8 columns (250mm × 4mm i.d.) using a mobile phase containing 0.2% (w/v) sodium acetate and 2.5% (v/v) glacial acetic acid in distilled water. A UV detector set at 313nm was used for quantitation. The method was applied to commercial toothpastes containing 5% potassium nitrate and yielded an average recovery of 100.1% with a relative standard deviation of 1.43%. Average recovery of nitrate and nitrite from spiked samples were 100.6% and 96.4%, respectively. The minimum detectable concentration for nitrite was 50 μg/g of toothpaste.