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The flavor of white wines is due to a complex mixture of many volatile compounds. These compounds have distinct physicochemical properties regarding, for example, polarity, volatility and odour impact. In this study, for isolation of free and glycosidically-bond volatile compounds, a head space solid-phase microextraction (HS-SPME) procedure was applied for sample preparation of white and red wines from Macedonia followed by separation and identification with GC-MS. Separation of the compounds was performed on a Carbowax column after the injection of the CRB-DVB-PDMS fiber in splitless mode. The liberation of the glycosidically-bond volatiles was perform by application of enzyme “Endozyme Aromatic” for “Temjanika” and “AR 2000” for the rest of examined wines. The main gropes of volatile compounds in Temjanika and Muscat wines produced from Muscat de Frontignan grape variety were terpenes especially limonene, p-cymene, linalool, gernaiol, citronellol and for other wines produced from red grape variety such as Vranec and Merlot, the most abundant compounds were alcohols, esters and fatty acids. Statistical analyses confirmed that the effect of enzymatic treatment for the examined wines was more significant than the varieties of grapes from which the wines were produced.