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…

CHARACTERIZATION OF ENOLOGICAL OAK TANNIN EXTRACTS BY MULTI-ANALYTICAL METHODS APPROACH

Oak tannin extracts are commonly used to improve wine properties. The main polyphenols found in oak wood extracts are ellagitannins¹ that release ellagic acid upon hydrolysis and comprise numerous structures². Moreover, oak tannin extracts contain other compounds giving a complex mixture. Consequently, the official OIV method based on gravimetric analysis of the tannin fraction adsorbed on polyvinylpolypyrrolidone is not sufficient to describe their composition and highlight their chemical diversity.

LARGE-SCALE PHENOTYPIC SCREENING OF THE SPOILAGE YEAST BRETTANOMYCES BRUXELLENSIS: UNTANGLING PATTERNS OF ADAPTATION AND SELECTION, AND CONSEQUENCES FOR INNOVATIVE WINE TREATMENTS

Brettanomyces bruxellensis is considered as the main spoilage yeast in oenology. Its presence in red wine leads to off-flavour due to the production of volatile phenols such as 4-vinylphenol, 4-vinylguaiacol, 4-ethylphenol and 4-ethylguaiacol, whose aromatic notes are unpleasant (e.g. animal, leather, horse or pharmaceutical). Beside wine, B. bruxellensis is commonly isolated from beer, kombucha and bioethanol production, where its role can be described as negative or positive. Recent genomic studies unveiled the existence of various populations.

EXPLORING THE INFLUENCE OF S. CEREVISIAE MANNOPROTEINS ON WINE ASTRINGENCY AND THE IMPACT OF THEIR POLYSACCHARIDE STRUCTURE

Mannoproteins (MPs) are proteoglycans from the outmost layer of yeast cell walls released into wine during alcoholic fermentation and ageing on lees processes. The use of commercial preparations of mannoproteins as additives to improve wine stability with regards to the crystallization of tartaric salts and to prevent protein haze in the case of white and rosé wines is authorized by the OIV.
Regarding red wines and polyphenols, mannoproteins are described as able to improve their colloidal stability and modulate the astringent effect of condensed tannins. The latter interact with salivary proteins forming insoluble aggregates that cause a loss of lubrication in the mouth and promote a drying and puckering sensation. However, neither the interaction mechanisms involved in mannoproteins capacity to impact astringency nor the structure-function relationships related to this property are fully understood.

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.

TANNINS AND ANTHOCYANINS KINETICS OF EXTRACTION FROM ARINARNOA, MARSELAN AND TANNAT UNDER DIFFERENT WINEMAKING TECHNIQUES

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.