The total oil content of soyflakes, canola seed and wetmilled corn germ were determined by analytical supercritical fluid extraction (SFE) with carbon dioxide as the extraction solvent. Results obtained by SFE were in excellent agreement with those obtained by a conventional Soxhlet technique with organic solvents. The analytical‐scale SFE technique yielded average means within one standard deviation of the means derived from the organic solvent‐based methodology. Matrices containing both high and low oil content were successfully extracted with carbon dioxide at comparable precision to that obtained with the standard procedure. The supercritical fluid‐based technique appears to be a suitable replacement for traditional extraction methods with organic solvents, thereby potentially eliminating the costs associated with solvent disposal and exposure of laboratory personnel to toxic and flammable solvents.