The occurrence of 2-furaldehyde (F) and 5-hydroxymethyl-2-furaldehyde (HMF) in processed citrus juices is an indication of quality deterioration. A close relationship between flavor changes and F content exists, while HMF can give rise to browning reactions. Both F and HMF are formed during heat processing or storage at improper temperatures. The detection of these compounds becomes more and more important as aseptic processing and packaging of citrus juices are becoming widespread. Aseptic packaging allows higher temperatures during distribution and storage to be employed without microbial spoilage, but off-flavors develop as citrus products are exposed to these conditions. In this paper a method of determination by high performance liquid chromatography (HPLC) is described. The method is based on the formation of the 2,4-dinitrophenylhydrazones of carbonyl compounds and subsequent reversed-phase separation of these derivatives. Derivatization is carried out by utilizing an acidic solution of 2,4-dinitrophenylhydrazine in acetonitrile. Precipitation of the derivatives of carbonyl compounds is thus avoided, and direct injection of the sample into the HPLC system is allowed. The determination offers a high specificity and a detection limit of the order of 10-8 mol/l for both analytes. Recoveries from an orange juice spiked at different levels are quantitative. Reproducibility data are presented