Selenium is an element toxic in large quantities, but an essential trace metal for mammals, birds, and many bacteria. Selenium-containing food also contains sulfur, and the ratio of Se: S is over 1:1x104. Selenium can replace sulfur easily, and the interaction between selenium and sulfur occurs easily as well. In order to investigate the potential interaction of organoselenium and organosulfur compounds, a model reaction of selenomethionine, glucose and diallyl disulfide was performed, and volatile products generated were identified by GC/AED and GC/MS. Atomic emission detector is a powerful detector due to its high sensitivity, elemental selectivity, and the ability of multielement analysis. When coupled with GC, it is able to monitor the elemental composition of eluates directly with high elemental specificity, tolerate of non-ideal separation, the selectivity of plasma emission being able to overcome the interference from complex matrixes, and detect multi-element simultaneously for empirical and molecular formula determination.