Two analytical procedures based on headspace solid-phase microextraction (HS-SPME) and static headspace (SH) extraction were developed for the characterization of minor and major volatile compounds of jelly palm wine, respectively. Volatile compounds were quantitatively evaluated (GC-FID) and identified by GC/MS and gas chromatography-olfactometry (GC-O). SPME fiber type, sodium chloride addition, extraction time, and temperature were evaluated to optimize the minor volatile extraction using HS-SPME technique. Based on a previous extraction optimization, a divinylbenzene/carboxen/polydimethylsiloxane fiber was used for extraction at 35 °C for 45 min with continuous stirring. SH method was effective to determine major volatile compounds. Method performance was evaluated according to linearity (0.991–0.998), sensitivity LOD (0.03–0.3) and LOQ (0.1–1), precision as repeatability (6.5–10.9 %) and intermediate precision (7.2–10.3 %), and accuracy (86–96 %). The identified volatile compounds were mostly ester, which were associated, by GC-O analysis, to the main positive aroma descriptors of jelly palm wine. Finally, ethyl hexanoate was described as the natural aroma of this product.