Abstract: The objective of this study was to investigate the volatile flavor compounds of nkui, a Cameroonian food, using solid phase microextraction (SPME) and a two-dimensional gas chromatography time of flight mass spectrometry GC×GC-TOF-MS system. Using SPME, volatile compounds were extracted from nkui and analyzed by GC×GC-TOF-MS. The data retrieved revealed the presence of flavor volatiles including acids (20%), alcohols (4%), aldehydes (10%), aromatic compounds (4%), esters (7%), furans (4%), ketones (11%), terpenes and terpernoids (27%). Although the terpene compounds were the most predominant, an ester (linalyl acetate) had the highest percentage of 19%, conferring a sweet, green and citrus flavor. Results obtained from this study suggest that the characteristic flavor of nkui was due to the combination of different volatile flavor compounds, which contributed to its aroma. Considering the medicinal importance of these compounds, their presence positions nkui as a vital food source with health benefits and medicinal properties.