Arabica coffee was roasted in a Probat Type 1 Z at 180 °C for 7 minutes, compared to green coffee. The formation of certain aldehydes consistently occurs alongside the decomposition of lipid hydroperoxides during the roasting of Arabica coffee. The primary fatty acids in Arabica coffee—linoleic acid (C18:2), palmitic acid (C16:0), oleic acid (C18:1), and stearic acid (C18:0)—were analyzed through transesterification of the triacylglycerols. Fatty acids were derivatized using the BF₃–methanol method and quantified by gradient elution reversed-phase high-performance liquid chromatography (RP-HPLC). Several carbonyl compounds were also analyzed, including hydroxypentanal and heptatrienal, with concentrations of 57.45 µmol/mL and 224.80 µmol/mL, respectively. Based on calibration with hexanal, all other dominant compounds were present in similar concentration ranges, with maximum concentrations determined by LC-MS.