Résumé : This data article describes the analysis of volatile organic compounds(VOCs) in 44 samples of cocoa bean shells (CBS) obtainedfrom cocoa beans of diverse cultivars and collected in differentgeographical origins. The volatile compounds were extracted byheadspace solid-phase microextraction (HS-SPME) method andthen analyzed by gas chromatography coupled to a quadrupolemass spectrometry GC-qMS. The retention times, identificationand semi-quantification of 101 VOCs are reported. Data collectedon the volatile profile of CBS samples using E-nose analysis are alsoavailable. Additional data related to physicochemical characteristicsand color analysis for CBS samples are reported. Furtherinterpretation and discussion on these datasets can be found in therelated article entitled “Assessment of volatile fingerprint by HSSPME/GC-qMS and E-nose for the classification of cocoa beanshells using chemometrics” (Barbosa-Pereira et al., 2019).