Twenty nine samples of grape marc spirits, nineteen from Spain (Orujo) and ten from Italy (Grappas) were analyzed by GC–MS in order to determine their major volatile composition. The results obtained showed that Orujo samples contained significantly higher concentration of methanol, 2-butanol, ethyl acetate and ethyl lactate. Grappas were defined as distillate with low contribution of the majority volatile compounds, both from qualitatively and quantitatively point of view. This aspect has a notable interest because, in the case of single-varietal aromatic distillates, the contribution of the primary aroma will be more intense. 2-phenyl ethanol, hexenols, aldehydes and the majority of ethyl esters and acetates showed large variations of concentrations between the samples; consequently they could be the responsible of the particular characteristics in these grape marc distillates.