Gas chromatographic (GC) analysis in solution and head space solid-phase microextraction (SPME)-GC analysis of a sample of crude oil gave different results. The SPME technique allowed the identification of a larger number of components than by using usual GC-mass spectrometry (MS). The method failed within the range of C14-C25 where GC-MS in solution allowed to obtain more representative results; on the contrary, SPME allowed to obtain data on the presence of volatile compounds that can not be identified in GC-MS analysis in solution. Furthermore, in the range C8-C12, SPME allowed to identify approximately 30 compounds not shown in the GC-MS analysis in solution. SPME analysis showed the presence of some alkenes not identified in GC-MS analysis in solution. SPME-GC-MS can be used in the analysis of crude oil in contaminated soil.