The analysis of biocompatible polyurethanes is used to illustrate the feasibility of supercritical fluid extraction-supercritical fluid chromatography-mass spectrometry using a simple supercritical fluid chromatographic-mass spectrometric interface for the study of polymer additives. Consistent and, for the most part, representative mass spectra can be obtained in an analysis that takes less than an hour to complete. Off-line supercritical fluid extraction-gas chromatography-mass spectrometry and supercritical fluid extraction-supercritical fluid chromatography-flame ionization detection were used to characterize the extracted material.