A HPLC method for the determination of Usal (Aspartame hydrochloride, L-aspartyl-L-phenylalanine methyl ester hydrochloride) and its decomposition products was elaborated. Aspartic acid, phenylalanine, phenylalanine methyl ester, aspartyl-phenylalanine, phenylalanyl-aspartic acid, 5-benzyl-3,6-dioxo-2-piperazineacetic acid (DOP) and Usal were separated on Separon SI C-18. The mobile phase was: 0.5 M NaH2PO4 (pH 2.1) and methanol (85:15 v/v). The detection was carried out at 200 nm. The method for DOP determination was tested by the analysis of 10 types of soft drinks to which DOP was added. In two newly developed sorts of soft drinks sweetened with Usal the formation of DOP was followed during storage. The DOP increment after 34 days of storage reached 0.7 and 6 mg/l at 7 and 20 degrees C, resp. The method is also suitable for DOP determination in the sweetener itself.