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…

REGULATION OF CENTRAL METABOLISM IN THE LEAVES OF A GRAPE VINES VA- RIETAL COLLECTION ON A TEMPERATURE CLINE

Grape (Vitis vinifera) is one of the world’s oldest agricultural fruit crops, grown for wine, table grape, raisin, and other products. One of the factors that can cause a reduction in the grape growing area is temperature rise due to climate change. Elevated temperature causes changes in grapevine phenology and fruit chemical composition. Previous studies showed that grape varieties respond differently to a temperature shift of 1.5°C; few varieties had difficulties in the fruit development or could not reach the desired Brix level.

HOW TO EVALUATE THE QUALITY OF NATURAL WINES?

The movement of Natural wines has clearly increased in the last few years, to reach a high demand from consumers nowadays. Switzerland has not been left out of this movement and has created a dedicated association in 2021. This association has the ambition to develop a specific tasting sheet for natural wines. The study of the tasting notes shows that the olfactory description of wines is recent but predominant today. But wine is a product makes to be drunk and not (just) to smell it. Based on these findings, a new 100-point tasting sheet has been developed. The main characteristics are 1) an evaluation in the mouth before the description of the olfaction, 2) to give 50% of the points on the judgment for the mouth characteristics, 3) to pejorate the visual aspects only if the wine is judged as “not drinkable” and 4) to express personal emotions.

NEW METHOD FOR THE QUANTIFICATION OF CONDENSED TANNINS AND OTHER WINE PHENOLIC COMPOUNDS USING THE AUTOMATED BIOSYSTEMS SPICA ANALIZER

Wine phenolic compounds are important secondary metabolites in enology due to their antioxidant and nutraceutical properties, and their role in the development of color, taste, and protection of wine from oxidation and spoilage. Tannins are valuable phenolic compounds that contribute significantly to these wine properties, especially in mouthfeel characteristics; however, tannin determination remains a significant challenge, with manual and time-consuming methods or complex methodologies. The purpose of this study is to propose a novel method for quantifying condensed tannins in finished wine products.

ACCUMULATION OF GRAPE METABOLITES IS DIFFERENTLY IMPACTED BY WATER DEFICIT AT THE BERRY AND PLANT LEVELS IN NEW FUNGUS DISEASE-TOLERANT GENOTYPES

The use of new fungus disease-tolerant varieties is a promising long-term solution to better manage chemical input in viticulture, but unfortunately little is known regarding these new hybrids fruit development and metabolites accumulation in front of abiotic stresses such as water deficit (WD). Thus, prior to the adoption of such varieties by the wine industry in Mediterranean regions, there is a need to consider their suitability to WD.

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.