Gas chromatography/mass spectrometry (GC/MS) is a powerful analytical technique that is widely used to detect and characterize low molecular weight compounds across diverse research fields, including food science. By combining the separation ability of a gas chromatograph with the identification capability of a mass spectrometer, GC/MS analysis allows the identification of a wide range of compounds. This technique offers several advantages, including fast, able to provide high resolution results, sensitive, inexpensive, and reliable when appropriate methods and components are applied. The selection of appropriate methods, instrument components, and analysis modes is critical to ensure that analysis objectives are met. Careful selection can significantly influence the accuracy and reliability of the results. Therefore, this chapter provides an overview of general considerations for method development in GC/MS analysis, highlighting the characteristics and roles of major components in analytical performance.