This paper describes the evaluation of purine alkaloids and diketopiperazines (DKPs) contents in 24 samples of processed non-alkalinized cocoa powder. The chemical data obtained were related to sensory evaluation and subjected to analysis of variance. During cocoa roasting, the content of DKPs can be increased, resulting in a negative influence on the sensorial quality of cocoa. A pronounced bitter metallic taste can originate from some of these compounds, and becomes stronger when these DKPs are combined with purine alkaloids. The cocoa roasting process at different temperatures (125, 130, 135, 140 and 145 7C) and durations (3, 10, 16 and 20 min) was evaluated by measuring the flavour indices, formol numbers and DKP contents in 24 samples of cocoa powder. The addition of reducing sugars was also evaluated in the same industrial processes in 27 other samples of cocoa powder. The higher the roasting temperature of the cocoa was, the more elevated the flavour index became, except at temperatures up to 140 7C, where DKPs were generated in large proportions.