A procedure has been developed for the GC-MS analysis of the aromas released in fast acid hydrolysis of precursor fractions from grape musts and skins. Different sorbents for the extraction of the precursors were compared. The best results were obtained with LiChrolut EN polymeric resins which displayed two and six-fold more extraction capacity than Amberlite XAD-2 resins and C18 sorbents, respectively. C18 sorbents are more suitable for selective extraction of less polar precursors. The initial version of the method was imprecise and so the imprecision of the different steps was assessed. The maceration of the solid parts and the liquid-liquid extraction of the aromas released in the acid hydrolysis proved to be the critical steps. Greater crushing of the solid parts and solid-phase extraction (SPE) instead of liquid-liquid extraction (LLE) improved reproducibility. In the method finally proposed about 100 aromatic components belonging to four large groups (lipid derivatives, shikimic acid derivatives, norisoprenoids and terpenes) were determined with good reproducibility. Important aroma compounds, such as cis-rose oxide or wine lactone were detected in non-Muscat grapes.