Gas chromatography/mass spectrometry (GC/MS) is useful in analyzing mixtures of organic compounds. This article commences with a description of the principles of mass spectrometry and gas chromatography. It provides information on the procedures of mass spectrum interpretation, and describes the experimental procedure of and sample preparation for GC/MS. The article also discusses complementary techniques, such as high-performance liquid chromatography/mass spectrometry and mass spectrometry/mass spectrometry, and concludes with the applications of GC/MS.