The cocoa shell is a residue of low commercial value, which represents an alternative for obtaining substances of added value for the food and pharmaceutical industry. Substances of interest in the shell include fat and methylxanthines (theobromine and caffeine). In order to obtain the extraction behavior with supercritical CO2, a 23 factorial design was proposed with six central points, taking dynamic extraction into consideration. The following factors were involved: pressure (2,000–6,000 psi), temperature (313–333 K), and time (30–90 min). The obtained yield was between 3.66% and 15.30%. Fat was the substance that was extracted most effectively (94.73%). Caffeine demonstrated variability in the residue, with at least six treatments that exceeded a removal rate of more than 90%, while it was practically impossible to extract theobromine. The difference with regard to the extraction of theobromine may be attributed to its low solubility. Characterization using FT–IR showed the modifications before and after the process, providing clear evidence of the changes corresponding to the fat at 2,924, 2,854 and 1,745 cm−1. The results presented establish the basis for the extraction of substances such as fats and methylxanthines from a cocoa shell with the use of CO2.
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