Abstract In this study, a headspace solid-phase microextraction method was established for extracting volatiles from cocoa powders sourced from five regions, including both natural and alkalized variants, with subsequent characterization performed via gas chromatography–mass spectrometry. Optimization experiments demonstrated that the optimal extraction efficiency was achieved when the samples were equilibrated at 77 °C for 32 min and then subjected to extraction for 72 min. Under these conditions, 104 volatile compounds were extracted from the cocoa powder samples, including nine alcohols, 16 aldehydes, 11 ketones, 11 acids, 14 esters, 20 pyrazines, six pyrroles, four furans, and 13 other compounds. Combined with multivariate statistical analysis, odor activity value analysis identified 21 compounds as the key differential substances for distinguishing these cocoa powders.
Wu et al. (2026) studied this question.