Volatile profile and aroma potential of tropical Syrah wines elaborated in different maturation and maceration times using comprehensive two-dimensional gas chromatography and olfactometry.  The influence of different combinations of Syrah grape maturation degree (19, 21 and 23 °Brix) and maceration times (10, 20 and 30 days) on the volatile profile and aroma potential was evaluated for the first time through different chromatographic platforms (GC × GC/TOFMS, GC-O-OSME, GC-FID and GC/MS). GC × GC/TOFMS analyses resulted in 145 identified compounds and among these 29 were determined to be the most important for wine differentiation. The aroma compounds allowed the discrimination of Syrah wines made with grapes macerated for a shorter time (ten days) due to the higher levels of volatile compounds. The evaluation of these wines through GC-O-OSME together with GC-FID, MS resulted in the designation of 19 °Brix as the most appropriate grape maturation degree to obtain a greater number of volatiles with pleasant odor and higher intensity and persistence. GC × GC/TOFMS allowed five and six co-elutions to be resolved, involving, respectively, ten and twelve important wine compounds.