This experiment combines analytical techniques of solid phase microextraction and gas chromatography-mass spectrometry with easily relatable and accessible plant volatile chemistry (floral and vegetative scents of local/available plants). The biosynthesis and structure of these chemicals are of interest in the areas of organic chemistry, biochemistry, and molecular biology. This laboratory exercise is well-suited for a broad range of cross-disciplinary topics in chemistry and biology courses. The methods described here could be used to expose undergraduate chemistry students to broad aspects of biological volatile chemistry in plants, and alternatively, to expose undergraduate biology students to analytical chemistry techniques useful in the study of plant biology and plant-insect interactions.