Early-Stage Electrochemical Kinetics of Agave Distillates: Impact of Barrel Toasting on Polyphenol Extraction Dynamics

Abstract

The maturation of distilled spirits in wooden barrels is a critical process that defines the sensory profile and quality of the final product, primarily through the release of polyphenols and flavonoids. In this study, the early extraction kinetics of these compounds in agave distillates were investigated using laboratory-scale barrels (5 L) with three toasting levels: light (185 °C/60 s), medium (210 °C/90 s), and intense (235 °C/120 s). The barrels were characterized by FTIR and Raman spectroscopy (SEM), as well as Scanning Electron Microscopy to correlate the chemical structure of the wood with the release of phenolic compounds. For this purpose, the Electrochemical Color Index (ECI), representative of polyphenols and flavonoids, was monitored daily for over 60 days. Results showed no statistically significant differences (p > 0.05) among the toasting levels. On the other hand, the observed kinetics exhibited four characteristic phases: (i) a linear increase during the first week due to the extraction of the most exposed compounds, (ii) a partial decrease in the second week associated with the re-adsorption of extracted compounds onto active sites remaining available on the barrel surface, (iii) a pseudo-steady state up to day 60, and finally, (iv) a subsequent linear increase. These findings provide scientific evidence supporting the official standards for the classification of aged distillates, since at least 60 days are required to condition the barrel surface to achieve a balanced extraction of polyphenols and flavonoids. The results highlight ECI as a robust and sensitive tool for monitoring the early maturation of agave distillates. Furthermore, the proposed approach not only offers complementary analytical criteria but also contributes to supporting the regulatory definitions of the reposado category, providing a practical framework for process standardization.