Abstract Dimethyl sulfide (DMS) is an important aroma and flavor constituent of a variety of food products, including many vegetables, wine, beer, and milk. Analysis of DMS in food products has been done almost exclusively through headspace analysis. Headspace analysis is not as appropriate for DMS analysis as it is for other compounds because gaseous DMS is so volatile that it cannot be properly contained, even in a sealed vessel. The following method avoids the problems of headspace analysis and, in addition, is compatible with the use of automatic samplers for gas chromatography. Extraction and GC analysis of powdered corn samples supplemented with purified DMS gave recovery rates of near 100%. Analysis for DMS content of different genotypes of corn harvested at different maturities was conducted, and significant differences were found both between genotypes on the same harvest date and within genotypes for different harvest dates.