Square-wave voltammetry (SWV) was investigated as a potential analytical tool for quantitation of unsaturated fatty acid oxidation in edible oils exposed to high heat. A traditional linear regression calibration curve and a novel single-point calibration method were used to quantitate linoleic acid in oxidized oil samples. These methods were compared to a standard method for fatty acid analysis via gas chromatography flame ionization detection (GC-FID). Both GC-FID and SWV methods were able to detect a decrease in linoleic acid concentration for heated oil samples. SWV methods routinely calculated higher linoleic acid concentrations compared to GC-FID analysis. A novel finding is that SWV oxidation peak intensities, which are associated with electroactive compounds, decrease in intensity over time for peaks below 1.0 V and increase for peaks above this voltage. These findings represent a step forward in electrochemical characterization of heated oils in addition to further advancing opportunities for electrochemical oil quality screening.