This article briefly describes the capabilities of gas chromatography/mass spectrometry, which is used to qualitatively and quantitatively determine organic (and some inorganic) compound purity and stability and to identify components in a mixture. The discussion covers in more detail gas chromatography/mass spectrometry (GC/MS) instrumentation, interpreting mass spectra, GC/MS methodology, and GC/MS advances. Sample preparation, which is very important in GC/MS to avoid erroneous data and to minimize maintenance and troubleshooting of the instrument, is also discussed. Further, the article highlights the state of the art in the MS detector technology.