AbstractThe direct combination of gas‐liquid chromatography with mass spectrometry represents one of the most powerful techniques available for the analysis of complex mixtures of lipids. Principal advantages are the extremely small amounts of material required, the relative speed of analysis, and the wealth of molecular structural information available. The ability to record rapidly several mass spectra of one emerging chromatographic peak may also frequently be of use in detecting impurities, unresolved mixtures, or thermal decomposition of the sample. In the development of new gas chromatographic analytical procedures, the combination instrument may frequently prove highly useful for following chemical reactions in the preparation of new types of derivatives for GLC.