Colombia is the third largest coffee producer, however, the coffee has not been widely studied, especially in terms of the metabolites produced during natural fermentation. To understand the sensorial correlation between chemical profile of volatile and nonvolatile components and final cup quality test. This work present the results of modification of natural fermentation from dry to wet, in three different municipalities in Nariño state. During 24 h were monitored the pH, temperature, Brix degree, sugar consumption. Samples were taken each 6 h and molecules were characterized using HPLC and GC-MS. From the results, was found a direct correlation between sensorial SCAA test and the formation of organic acids and volatile compounds. The chemical characterization showed the production of organic acids such as lactic, citric succinic and acetic, accompanied by 67 minor volatile compounds detected by GC-MS. The implementation of wet fermentation increases final cup test, mainly related to metabolites produced.