Grape products are really important in the cultural and dietary Italian traditions. Oenological products have been largely studied since the early ’70s, even if the lack of biochemical and microbiological knowledge and poor sensitivity of the analytical techniques prevent from carrying on a deep studies on sulfur compounds. The topic discussed in the present work is the development of HS-SPME/GC-MS methods to quantify fermentative sulfur compounds (i.e. molecules produced both by yeast metabolisms from amino acidic precursors and via chemical reactions from other sulfur compounds) and the following application of these procedures on still wines, sparkling wines and distillates (e.g. Italian Grappa). 13 and 10 sulfur compounds were quantified in still and sparkling wines and Grappas, respectively. Influence of variety, aging, yeast strain and other technological practices on the level of these fermentative sulfur compounds was also investigated.