Impact of Barrel Toasting on Ellagitannin Composition of Aged Cognac Eaux-de-Vie.

It is well established that C-glucosidic ellagitannins contribute to wine quality, and new forms of ellagitannins have been found recently in cognac eaux-de-vie. The contribution of some ellagitannin-derived spirit compounds to eaux-de-vie taste has been demonstrated recently. However, there is a gap in our knowledge of the content, composition, and evolution of C-glucosidic ellagitannins in this matrix. Indeed, the quantification of these compounds and their evolutionary compounds have never before been researched in cognac eaux-de-vie. Thus, the aim of this study was not only to quantify these compounds, but also to study their kinetics and to observe how they are impacted by barrel toasting. For this purpose, barrels representing eight different toasting levels were used to age the same eau-de-vie during the first 18 months. Ellagitannin quantification was carried out by HPLC-Triple quadrupole. The results showed that the evolutionary trend of the eight ellagitannins is the same for all eight types of barrel toasting. The maximum concentrations of C-glucosidic ellagitannins were found after 3 months of aging (up to 23 mg/L) before decreasing to 18 months (9.7 mg/L), whereas ellagitannin-derived spirit compound concentrations increased throughout aging (up to 130.9 mg/L). In addition, barrel toasting had such an impact on ellagitannin content that barrels could be differentiated according to their levels. Eaux-de-vie in barrels with high toasting were lower in ellagitannins concentrations.

Identification, quantitation and sensory contribution of new C-glucosidic ellagitannin-derived spirit compounds.

Ellagitannins are the main extractible phenolic compounds in oak wood. They can be extracted by eaux-de-vie aging in barrels but rapidly undergo chemical transformations, such as hydrolysis, reduction, oxidation, or even substitution reactions. Given gaps in knowledge about their composition in spirits, the goal of this work was to explore ellagitannin behavior during Cognac eaux-de-vie aging and search for new C-glucosidic ellagitannin-derived compounds. A purification protocol was followed to isolate the new formed compounds. UPLC-UV-Q-ToF and NMR spectroscopy were used to characterize a new C-glucosidic ellagitannin, named brandy tannin B. Two new forms of whiskey tannins were also isolated. The new compound, Brandy tannin B along with ß-1-O-ethylvescalagin and ß-1-O-ethylvescalin, and whiskey tannins were identified and quantified for the first time in Cognac eaux-de-vie. In addition, the organoleptic impact of brandy tannin B was evaluated. This work brings new insights into ellagitannin composition and their contribution to spirit quality.

Validation of a mass spectrometry method to identify and quantify ellagitannins in oak wood and cognac during aging in oak barrels.

Ellagitannins are the main extractible phenolic compounds in oak wood; the monomers vescalagin and castalagin, lyxose/xylose-bearing monomers grandinin and roburin E, dimers roburins A and D and lyxose/xylose-bearing dimers roburins B and C are the principal ones. These compounds are responsible for the high durability of wood and may contribute to the organoleptic quality of wines and spirits (color, astringency, bitterness). Despite their importance, their presence and forms in distilled spirits are not well known. The aim of this work was therefore to develop and validate a method to identify and quantify oak wood ellagitannins in Cognac using high liquid chromatography-triple quadrupole (LC-QQQ) analysis. The method was validated using vescalagin as the standard and by studying sensitivity, linearity in working range, intraday repeatability, and intraday precision in order to quantify individual ellagitannins in this complex matrix.