¹Genetris Danismanlik, Mersin, Türkiye DOI : 10.29228/jrp.858 This study investigated the composition of the aroma substances and the physicochemical properties of lyophilized coffee produced from Ecuador Arabica and robusta coffee beans. In the present study, we propose a fast method of analyzing volatile compounds in coffee using the headspace solid phase extraction method (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS). According to the results, 25 aroma compounds were detected in coffee, the most important of which are 2-acetylfuran, 2-furanmethanol, 2,3-dimethylpyrazine, 2,3,5-trimethylpyrazine, and 2-methoxy-4-vinylphenol. As is known, furans and pyrazines are associated with "roasted, cocoa, coffee, and hazelnut" odours. The most important organic acids detected in the study are citric, maleic, and succinic. Keywords : coffee; volatile compounds; caffeine; HS-SPME; organic acids