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In this study, four underutilized spices (fruit and ulb of Aframomum sulcatum, fruit of Xylopia africana, and bark of Hypodaphnis zenkeri) were analyzed for their physical properties, nutrients composition, and profile of volatile compounds using standard analytical methods. The protein, fat, sugar, and dietary fiber contents were analyzed. The spices were revealed to be a good source of essential amino acids and fatty acids including pentadecanoic acid. Several minerals (Mn, Mg, Ca, Fe, and K) of nutritional importance were found at various proportions. Electronic nose analysis revealed the presence of fifty-six different compounds, belonging to ten major classes (phenylpropenes, acids, alcohols, aldehydes, esters, ketones, terpenes, pyrazine, sulfur-containing compounds, and ether) and also some flavor-characterizing compounds responsible for a variety of sensory descriptors. Bioactive volatile compounds like terpinen-4-ol, dimethyl trisulphide, and P-cymene were found in these spices, which can be further applied in the development of functional foods and nutraceuticals.