Aspartame (Apt), Acesulfame-K (Ace-K) low-calorie, high-potency artificial sweeteners are currently used in beverages and dietary food and drinks. Their increased application in food and drink products has given a new impetus to develop fast and accurate methods for their determination. Absorption spectra of Asp, Caf, Ace-K and BA strongly overlap. Therefore a direct determination of these analytes in quaternary mixture is impossible without a separation step. In order to overcome this difficulty partial least squares (PLS) method has been proposed.