Gas chromatography–mass spectrometry (GC–MS) is a powerful analytical tool for detection, identification, and quantification of many volatile organic compounds. However, many colleges and universities have not fully incorporated this technique into undergraduate teaching laboratories despite its wide application and ease of use in organic chemistry. In this article, a set of experiments are provided to educators for the purposeful integration of the GC–MS technique into undergraduate organic chemistry laboratories. The laboratories provide students experimental opportunities to use GC–MS as the main analytical tool for (a) identification and quantification of major and minor product(s) formed in three common organic synthesis reactions and (b) extraction, separation, and identification of multiple natural products found in fruits and vegetables.