terclim by ICS banner
IVES 9 IVES Conference Series 9 USE OF 13C CP/MAS NMR AND EPR SPECTROSCOPIC TECHNIQUES TO CHARACTERIZE MACROMOLECULAR CHANGES IN OAK WOOD(QUERCUS PETRAEA) DURING TOASTING

USE OF 13C CP/MAS NMR AND EPR SPECTROSCOPIC TECHNIQUES TO CHARACTERIZE MACROMOLECULAR CHANGES IN OAK WOOD(QUERCUS PETRAEA) DURING TOASTING

Abstract

For coopers, toasting process is considered a crucial step in barrel production during which oak wood (Q. petraea) develops several aromatic nuances released to the wine during its maturation. Toasting consists of applying different degrees of heat to a barrel for a specific period. As the temperature increases, thermal degradation of oak wood structure produces a huge range of chemical compounds. Many studies have identified the main key aroma volatile compounds (whisky-lactone, furfural, eugenol, guaiacol, vanillin). However, detailed information on how the chemical structure of oak wood degrades with increasing toasting level is still lacking.

In this study, we characterised the structural changes of the main components (cellulose, hemicellulose and lignin) of oak wood staves subjected to heat treatments (non-toasted to 240 °C) by cross-polarisation/magic angle spinning nuclear magnetic resonance (CP/MAS NMR, 800 MHz) and electron para-magnetic resonance (EPR, X-band) spectroscopy techniques applied to solids. Furthermore, the results will be compared to those obtained by quantitative GC-MS (EI) analysis of oak wood volatile compounds generated by the same heat treatments. The 13C CP/MAS NMR data highlighted concomitant phenomena of demethoxylation and depolymerisation of syringyl units leading to the formation of guaiacyl units and the release of monomer units. EPR results revealed the same phenomena and led us to hypothesize that the nature of the radical formed evolved during toasting from syringyl to guaiacyl form. Our results are consistent with data on others wood species and confirm that 200 °C is a threshold temperature above which degradation of the macromolecular structure leads to the formation of radicals and volatile compounds. Overall, the study offers interesting perspectives for the application of spectroscopic techniques, particularly EPR spectroscopy, to monitor radical formation during barrel aging and, consequently, to assess the oxidative stability of wine.

DOI:

Publication date: February 9, 2024

Issue: OENO Macrowine 2023

Type: Poster

Authors

Marie Courregelongue 1,2,3, Mathieu Duttine ⁴, Axelle Grélard ⁵, Alexandre Pons 1,2,3

1. Univ. Bordeaux, Bordeaux INP, INRAE, OENO, UMR 1366, ISVV, F-33140 Villenave d’Ornon, France
2. Bordeaux Sciences Agro, F-33170 Gradignan, France
3. Seguin Moreau Cooperage, ZI Merpins, F-16103 Cognac, France
4. Univ. Bordeaux, CNRS, Bordeaux INP, ICMCB, UMR 5026, F-33600 Pessac, France
5. Univ. Bordeaux, CNRS, Bordeaux INP, CBMN, UMR 5248, IECB, F-33600 Pessac, France

Contact the author*

Keywords

oak wood, thermal degradation, macromolecular components, aroma compounds

Tags

IVES Conference Series | oeno macrowine 2023 | oeno-macrowine

Citation

Related articles…

EFFECT OF FUMARIC ACID ON SPONTANEOUS FERMENTATION IN GRAPE MUST

Malolactic fermentation (MLF)¹, the decarboxylation of L-malic acid into L-lactic acid, is performed by lactic acid bacteria (LAB). MLF has a deacidifying effect that may compromise freshness or microbiological stability in wines² and can be inhibited by fumaric acid [E297] (FA). In wine, can be added at a maximum allowable dose of 0.6 g/L³. Its inhibition with FA is being studied as an alternative strategy to minimize added doses of SO₂⁴. In addition, wine yeasts are capable of metabolizing and storing small amounts of FA and during alcoholic fermentation (AF).

RED WINE AGING THROUGH 1H-NMR METABOLOMICS

Premium red wines are often aged in oak barrel. This widespread winemaking process is used, among others, to provide roundness and complexity to the wine. The study of wine evolution during barrel aging is crucial to better ensure control of wine quality.
¹H-NMR has already been proved to be an efficient tool to monitor winemaking process [1]. Indeed, it is a non-destructive technique, it requires a small amount of sample and a short time of analysis, yet it provides clues about several chemical families.

WHICH IMPACT FOR PROANTHOCYANIDIC TANNINS ON RED WINE FRUITY AROMA? SENSORY AND PHYSICOCHEMICAL APPROACHES

Previous research on the fruity character of red wines highlighted the role of esters. Literature provides evidence that, besides these esters, other compounds that are not necessarily volatiles may have an important impact on the overall aroma of wine, contributing to a modulation of its global aromatic expression. The goal of this work was to assess the olfactory consequences of a mixture between esters and proanthocyanidic tannins, through sensory and physico-chemical approaches.
Sensory analysis of numerous aromatic reconstitutions, including triangular tests, detection thresholds, and sensory profiles, were conducted in order to evaluate the sensory impact of tannins on red wine esters perception.

IMPACT OF MINERAL AND ORGANIC NITROGEN ADDITION ON ALCOHOLIC FERMENTATION WITH S. CEREVISIAE

During alcoholic fermentation, nitrogen is one of essential nutrient for yeast as it plays a key role in sugar transport and biosynthesis of and wine aromatic compounds (thiols, esters, higher alcohols). The main issue of a lack in yeast assimilable nitrogen (YAN) in winemaking is sluggish or stuck fermentations promoting the growth of alteration species and leads to economic losses. Currently, grape musts are often characterized by low YAN concentration and an increase of sugars concentration due to global warming, making alcoholic fermentations even more difficult. YAN depletion can be corrected by addition of inorganic (ammonia) or organic (yeast derivatives products) nitrogen during alcoholic fermentation.

ASSESSMENT OF GRAPE QUALITY THROUGH THE MONITORING OFPHENOLIC RIPENESS AND THE APPLICATION OF A NEW RAPID METHOD BASED ON RAMAN SPECTROSCOPY

The chemical composition of grape berries at harvest is one of the key aspects influencing wine quality and depends mainly on the ripeness level of grapes. Climate change affects this trait, unbalancing technological and phenolic ripeness, and this further raises the need for a fast determination of the grape maturity in order to quickly and efficiently determine the optimal time for harvesting. To this end, the characterization of variety-specific ripening curves and the development of new and rapid methods for determining grape ripeness are of key importance.