Headspace solid phase microextraction (SPME), using a Carboxen-polydimethylsiloxane fiber, was compared with headspace entrainment on Tenax TA, as a means of examining the aroma constituents of cooked beef. Extracts were analyzed using gas chromatography-mass spectrometry. Headspace entrainment on Tenax extracted higher amounts of most volatiles, particularly low-boiling compounds. However, polar volatiles, such as hydroxyfuranones and hydroxyketones, were present at higher levels in the SPME extracts. Some components were present only in the SPME extracts, including norfuraneol, furaneol, and cyclotene, which are key Maillard reaction intermediates.