Solid-phase microextraction (SPME)-gas chromatography-mass spectrometry was used to identify the cuticular hydrocarbons of the subterranean termite Coptotermes formosanus Shiraki. Headspace SPME and direct contact SPME methods were evaluated and compared to the hexane extraction method. Variables, such as temperature, time, number of termites, condition of the termites, and the type of SPME fiber were evaluated. Methods were refined to increase the reproducibility as well as the sensitivity. Both SPME methods were successfully used for the identification of all the major termite cuticular hydrocarbons. Using the headspace SPME method, other compounds of interest could also be identified, such as fatty acids. Using the direct contact SPME method, termites could be repeatedly studied over time to monitor chemical changes.