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…

INOCULATION OF THE SELECTED METSCHNIKOWIA PULCHERRIMA MP1 AS A BIOPROTECTIVE ALTERNATIVE TO SULFITES TO PREVENT BROWNING OF WHITE GRAPE MUST

Enzymatic browning (BE) of must is caused by polyphenol oxidases (PPOs), tyrosinase and laccase. Both PPOs can oxidize diphenols such as hydroxycinnamic acids (HA) to quinones, which can later polymerize to form melanins [1], which are responsible of BE in white wines and of oxidasic haze in red wines. SO₂ is the main tool used to protect must from BE thanks to its capacity to inhibit PPOs [2]. However, the current trend in winemaking is to reduce and even eliminate this unfriendly additive. Among the different possible alternatives for protecting must against BE, the inoculation with a selected Metschnikowia pulcherrima MP1 is without any doubt one of the most promising ones.

ENRICHMENT OF THE OENOLOGICAL MALDI-TOF/MS PROTEIN SPECTRA DATABASE FOR RELIABLE OENOLOGICAL YEAST AND BACTERIA IDENTIFICATION

The Matrix Assisted Laser Desorption/Ionization–Time-Of-Flight Mass Spectrometry (MALDI-TOF MS) technology is commonly used in food and medical sector to identify yeast or bacteria species isolated from a nutritive culture media. Since a decade, brewery and oenology industries have been attracted to this method which combines fast analysis times, reliability and low cost of analysis. Briefly, this method is based on the comparison of the MALDI-TOF/MS protein spectra of an isolated colony of yeast or bacteria with those contain in a manufacturer’s reference protein spectra database. Initiated in 2015, the creation of the first oenological mass spectra database has proved to be essential for increase quality of species identification.

DETERMINATION OF MINERAL COMPOSITION IN CV. TERAN (VITIS VINIFERA L.) RED WINE AFFECTED BY PRE-FERMENTATIVE MASH COOLING, HEATING, SAIGNÉE TECHNIQUE AND PROLONGED POST-FERMENTATIVE MACERATIONS

This study aimed to determine mineral composition in red wine obtained from cv. Teran (Vitis vinifera L.), autochtonous Croatian grape variety. Six different vinification treatments, including the control treatment (7-day standard maceration), were performed to study the effects of: 48-hour pre-fermentative mash cooling (8 °C) followed by prolonged post-fermentative maceration of 13 days (C15), 28 days (C30), and saignée technique (juice runoff) proceeded with prolonged post-fermentative maceration of 13 days (CS15); and effect of 48-hour heating (50 °C) followed by prolonged post-fermentative maceration of 13 days (H15) and 28 days (H30) on macro- and microelements in wine.

THE EFFECT OF COPPER ON THE PRODUCTION OF VARIETAL THIOLS DURING THE ALCOHOLIC FERMENTATION OF COLOMBARD AND GROS MANSENG GRAPE JUICES

Nowadays, the rapid growth of vineyards with organic practices and the use of copper as the only fun-gicide against downy mildew raises again the question of the effect of copper on varietal thiols in wine, especially 3-sulfanylhexan-1-ol (3SH) and its acetate (3SHA). A few decades ago, several works indicated that the use of copper in the vineyard had a negative effect on the content of varietal thiols in Sauvignon blanc wines [1, 2]. However, these studies only considered the concentration of the reduced form (RSH) of varietal thiols, without quantifying the oxidised ones. For this purpose, we proposed to monitor both reduced and oxidised forms of varietal thiols in wine under copper stress during alcoholic fermentation to have a more complete picture of the biological and chemical mechanisms.

INFLUENCE OF WINEMAKING VARIABLES AND VINEYARD LOCATIONS ON CHEMICAL AND SENSORY PROFILES OF SOUTH TYROLEAN PINOT BLANC

Pinot Blanc, an important grape variety grown in some mountain areas of Northern Italy such as South Tyrol over the last decades, with its cultivation covering 10.3% of the total vineyards, has compatible climatic conditions (e.g. heat requirements) which are normally found in the geographical areas of the mountain viticulture [1,2,3,4]. Climatic changes are hastening the growth of this variety at higher elevations, particularly for the production of high quality wine.