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A gas chromatographic-mass spectrometric detection method for the analysis of diesel components in soil and water contaminated by semivolatile synthetic organic compounds is proposed. n-Alkanes in the range of C11-C22 are used as representative components for the analysis of diesel. It is shown that C3H7+ (MW 43) and C4H9+ (MW 57) have almost the same abundance with respect to their total ion chromatograms. Ions at m/z 43 and 57 are used as qualifier and target ions, respectively. It is demonstrated that none of the U.S. Environmental Protection Agency’s 8270 components (more than 100 semivolatile synthetic organic compounds) interfere with the analysis of diesel. The analysis of heavy oils (C23-C24) or fingerprints (C8-C34) in soil or water contaminated by semivolatiles can be performed in a similar way.