Lipid oxidation has long been recognized as a leading cause of quality deterioration in muscle foods and is often the decisive factor in determining food product storage life. Lipid oxidation generates a number of products, including volatile compounds, which are the major contributors to the development of rancid off-flavors and odors. Over the years, methodologies have been developed to quantify lipid oxidation products in muscle foods. This article reviews the analytical methods that have been used to quantify volatile compounds as indicators of lipid oxidation in muscle foods. The sampling methodologies of distillation/solvent extraction and headspace analysis, and isolation methods associated with gas chromatographic (GC) and high-performance liquid chromatography (HPLC) analyses are discussed. Within gas chromatographic methodologies, headspace (HS) sampling (static HS, dynamic purge-and-trap HS techniques, and solid-phase phase microextraction [SPME]) are addressed.