¹Genetris Danismanlik, Mersin, Türkiye DOI : 10.29228/jrp.2022.00 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