Nero d’Avola and Shiraz grapes were subjected to pre-fermentative cold maceration at 4°C for about 24 h in industrial winemaking, in order to evaluate the effects of the pre-treatment on aroma profile. The volatile compounds were identified by gas chromatography-mass spectrometry and grouped into 14 chemical families 4 and 9 months after bottling. Principal components analysis (PCA) plots of the volatile compounds showed clear separation among wines from the Shiraz and Nero d’Avola varieties. For instance, Shiraz wines were characterized along the PC1 axe by esters of organic acids, norisoprenoids and C6 alcohols, while Nero d’Avola wines were characterized by acetates and monoterpenic oxides and diols. Moreover, pre-treated samples showed significant (p < 0.05) changes in volatile compounds belonging mainly to ethyl esters of straight chain fatty acids, acetates and norisoprenoids. The sensorial analysis showed that cold maceration contributed to development of a different aroma profile during bottle maturation if applied on Nero d’Avola or Shiraz variety.