The unique properties of supercritical fluids have been successfully exploited in the development of novel hyphenated analytical techniques. Supercritical fluid extraction (SFE) followed by gas chromatography-mass spectrometry was used to characterize an intractable deposit from an internal combustion engine valve. Supercritical fluid chromatography-Fourier transform infrared spectroscopy (SFC-FTIR) was used to provide quantitative characterization of a range of polymeric surfactants. Finally, an example of SFE followed by SFC-FTIR is reported.