Chemically reducing species formed during phosphate ion catalyzed degradation of reducing sugars were directly quantified by titration with 2,6-dichloroindophenol (Tillman's reagent) and by measurement of open circuit electrical redox potentials. Both techniques demonstrated a time-dependent increased production of chemically reducing species in 0.1 M phosphate buffer at 100 degrees C and the increasingly negative redox potentials observed were consistent with the formation of reductones. Cyclic voltammetry (CV) was investigated in an attempt to generate and observe the sugar-derived highly reactive reducing species in situ. CV analysis of a model Amadori compound, N-(1-deoxyfructos-1-yl)piperidine, indicated oxidative waves consistent with reductone formation, but chemical instability of the oxidation products formed precluded the electrochemical detection of highly electrophilic reducing species such as reductones.