Abstract: A simple, specific and sensitive high-performance liquid chromatographic method was developed for the determination and detection of tocopherols in extracts by supercritical carbon dioxide. A supercritical carbon dioxide extraction with cosolvents procedure was used to concentrate tocopherols from the rapeseed deodorize distillates. The analyses were separated on a Zorbax C18 reversed-phase column using 98% methanol as mobile phase, UV detection at 292 nm and α-tocopherol as a standard. The calibration graphs of the method were linear. Results by APCI-MS2 experiments were consistent with outcomes from theories.