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…

THE INFLUENCE OF COMMERCIAL SACCHAROMYCES CEREVISIAE ON THE POLY-SACCHARIDES AND OTHER CHEMICAL PROFILES OF NEW ZEALAND PINOT NOIR WINES

Wine polysaccharides (PS) play an important role in balancing mouthfeel and stability of wine and even influence aroma volatility. Despite this, there is limited research into the effect of winemaking additives on the polysaccharide profile and other macromolecules of New Zealand (NZ) Pinot noir wine. In this study the influence of a selection of commercial S. cerevisiae strains on the chemical profile, including polysaccharides, of New Zealand Pinot noir (PN) wine was investigated. Research scale PN fermentations using five strains of commercially available S. cerevisiae (Lalvin EC1118 and RC212, Levuline BRG YSEO, Viallate Ferm R71 and R82) were undertaken. PS were qualified and quantified using HPLC-RID.

INSIGHTS ON THE ROLE OF GENES ON AROMA FORMATION OF WINES

Yeast secondary metabolism is a complex network of biochemical pathways and the genetic profile of the yeast carrying out the alcoholic fermentation is obviously important in the formation of the metabolites conferring specific odors to wine. The aim of the present research was to investigate the relative expression of genes involved in flavor compound production in eight different Saccharomyces cerevisiae strains.
Two commercial yeast strains Sc1 (S.cerevisiae x S.bayanus) and Sc2 (S.cerevisiae) and six indigenous S. cerevisiae strains (Sc3, Sc4, Sc5, Sc6, Sc7, Sc8) isolated during spontaneous fermentations were inoculated in Assyrtiko and Vidiano grape must.

HOLISTIC APPROXIMATION OF THE INFLUENCE OF SACCHAROMYCES STRAINS ON WINE AROMA PRECURSORS

Wine varietal aroma is the result of a mixture of compounds formed or liberated from specific grape-aroma precursors. Their liberation/formation from their specific precursors can occur spontaneously by acid catalyzed rearrangements or hydrolysis or by the action of the yeast enzymatic activities. The influence of yeast during fermentation on the production of these volatile compounds has been widely studied however, the effect of this influence during aging is not fully understood. In order to evaluate these processes several indirect strategies have been used to study aroma precursors although they are not useful to understand the chemistry of the process.

THE EFFECT OF BENTONITE FINING ON THE VOLATILE AND NON-VOLATILE PROFILE OF ITALIAN WHITE WINES

Marselan wines have an unusual high proportion of seed derived tannins from grapes having high proportions of skins, which are rich in tannins. But the causes behind this characteristic have not yet been identified. In vintage 2023 wines were made at experimental scale (9 kg by experimental unit) from Arinarnoa, Marselan and Tannat Vitis vinifera grape cultivars by traditional maceration, and by techniques aimed to increase the wine content in skin derived tannin: addition of extraction enzymes, addition at vatting of grape-skin enological tannins, or by extended maceration, known to increase the seed derived tannin contents of wines. Macerations were of 7 days, except in the extended macerations that were of 15 days.

TOWARDS THE SHELF-LIFE PREDICTION OF OLD CHAMPAGNE VINTAGES DEPENDING ON THE BOTTLE CAPACITY

Today, nearly one billion bottles of different sizes and capacities are aging in Champagne cellars while waiting to be put on the market. Among them, several tens of thousands of prestigious cuvees elaborated prior the 2000s are potentially concerned by prolonged aging on lees. However, when it comes to champagne tasting, dissolved CO₂ is a key compound responsible for the very much sought-after effer-vescence in glasses [1]. Yet, the slow decrease of dissolved CO₂ during prolonged aging of the most prestigious cuvees raises the issue of how long a champagne can age before it becomes unable to form CO₂ bubbles during tasting [2].