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This study is part of a wider project aiming to correlate the chemical composition of the coffee volatile fraction to its sensory properties with the end-goal of developing an instrumental analysis approach complementary to human sensory profiling. The proposed investigation strategy compares the chemical information concerning coffee aroma and flavor obtained with HS-SPME of the ground coffee and in-solution SBSE/SPME sampling combined with GC–MS to evaluate their compatibility with the cupping evaluation for quality control purposes. Roasted coffee samples with specific sensory properties were analyzed. The chemical results obtained by the three samplings were compared through multivariate analysis, and related to the samples’ sensory attributes. Despite the differences between the three sampling approaches, data processing showed that the three methods provide the same kind of chemical …