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…

EUGENOL AS QUALITY MARKER OF WINES AND SPIRITS FROM HYBRID VINES: IMPACT OF DIFFERENT WINEMAKING AND DISTILLATION PROCESSES

Eugenol, widely spread in various plants notably cloves, basil and bay, was identified too in wines from hybrid grapes without contact with oak wood. This aromatic molecule presents a strong spicy note of clove and also antifongic properties. Eugenol was described as an endogenous compound of Baco blanc, from the grapes to the spirits of Armagnac area. Moreover, this compound is a chemical marker of Baco blanc products quality. Influences of harvest time and different winemaking processes (settling, use of enzymatic preparations, lees content and stock time before distillation) on Baco blanc wine eugenol contents were explored using a two-levels full factorial Design of Experiments (DoEs).

IMPACT OF NEW BIO STIMULANTS ON GRAPE SECONDARY METABOLITES UNDER CLIMATE CHANGE CONDITIONS

In a context of climate change and excessive use of agrochemical products, sustainable approaches for environmental and human health such as the use of bio stimulants in viticulture represent a potential option, against abiotic and biotic threats. Bio stimulants are organic compounds, microbes, or a combination of both, that stimulate plant’s vital processes, allowing high yields and good quality products. In vines, may trigger an innate immune response leading to the synthesis of secondary metabolites, key compounds for the organoleptic properties of grapes and wines.

FLAVONOID POTENTIAL OF MINORITY RED GRAPE VARIETIES

The alteration in the rainfall pattern and the increase in the temperatures associated to global climate change are already affecting wine production in many viticultural regions all around the world (1). In fact, grapes are nowadays ripening earlier from a technological point of view than in the past, but they are not necessarily mature from a phenolic point of view. Consequently, the wines made from these grapes can be unbalanced or show high alcohol content. Dramatic shifts in viticultural areas are currently being projected for the future (2).

INVESTIGATION OF FILM COATINGS AS A PROTECTIVE LAYER IN REDUCING THE ABSORPTION OF SMOKE PHENOLS INTO PINOT NOIR GRAPES

Wine grapes exposed to wildfire smoke have resulted in wines with burnt and ashy sensory characteristics¹, that are undesirable qualities in wine. In extreme wildfire events, this can lead to total loss of grape crop. Currently there are no effective solutions in the market to prevent the uptake of smoke compounds into grapes. In this study, previously developed innovative film coatings were tested to analyze their effectiveness in reducing smoke phenol absorption². Four different cellulose nanofiber-based film types were investigated.

CLIMATE CHANGE EFFECT ON POLYPHENOLS OF GRIGNOLINO GRAPES (VITIS VINIFERA L.) IN HILLY ENVIRONMENT

Current changes of ecoclimatic indicators may cause significant variation in grapevine phenology and grape ripening. Climate change modifies several abiotic factors (e.g. temperature, sunlight radiation, water availability) during the grapevine growth cycle, having a direct impact on the phenological stages of the grapevine, modulating the metabolic profile of berries and activating the synthesis and accumulation of diverse compounds in the skin of berries, with consequences on the composition of the grapes.
The influence exerted by different meteorological conditions, during three consecutive years (2020-2022) on secondary metabolites such as the polyphenolic profile of Grignolino grapes was investigated. The samples were collected from three vineyards characterized by different microclimatic conditions mainly related to the vineyard aspect and to a different age of the plants.