Macrowine 2021
IVES 9 IVES Conference Series 9 Validation of a high-throughput method for the quantification of volatile carbonyl compounds in wine and its use in accelerated ageing experiments

Validation of a high-throughput method for the quantification of volatile carbonyl compounds in wine and its use in accelerated ageing experiments

Abstract

AIM: the aim of this study was the optimization and validation of a robust and comprehensive method for the determination of volatile carbonyl compounds (VCCs) in wines. The protocol was then applied to determine the evolution of VCCs in wines after accelerated ageing. VCCs are widely present in foods and beverages; their formation is due to chemical reactions and biological processes where oxygen plays a key role [1]. However, many of these are side transformations that highly affect the final aroma. The total package oxygen is usually negligible in bottled wines. However, that amount combined with temperature and light, can modify the oxidative status with a consequent loss in varietal aroma and an increase in off-flavors and defects [2]. At the same time, several carbonyls are related to pleasant scents so the winemaking of many oxidized wines like Madeira, Port, Vin Santo is tailored to emphasize their productions. We expect that a high-throughput method for the measure of the concentration of carbonyls could be added as a new quality control tool for the evaluation of a complete fermentation, correct winemaking style, and proper bottling and storage.

METHODS: Various white wines (cv. Gewürztraminer) and red wines (cv. Teroldego) were submitted to accelerated-ageing process. All bottles were opened under inert atmosphere inside a sealed hood and submitted to the accelerated-ageing procedure, according to Oliveira et. al. [3]. The extraction procedure was based on the protocol purposed by Moreira et. al. [4], upgraded with a fully automated sample preparation performed by a CTC-PAL3 autosampler. The sample was transferred from the 2 mL vial (kept at 5°C) to a 20 mL vial and then spiked with internal standard (IS) and derivatizing agent (PFBHA) solutions. After a 7 minutes derivatization at 45°C, the SPME extraction is performed at 40°C for 20 minutes. Finally, the fiber desorption takes place at 250°C for 4 min. GC-MS analysis was carried out using a TSQ Quantum XLS Ultra Triple Quadrupole GC-MS/MS using MRM acquisition. Calibration curves were acquired in matrix using a commercial white wine treated with activated carbon to remove odor active compounds. Acetone d6, 4-methyl-4-penten-2-one d10, Octanal d16 and 4-fluorobenzaldehyde were used as IS. As many as 56 VCCs were the analytes under investigation.

RESULTS: all compounds showed a good linearity spanning from approximately 0.1 to 50 µg/L (R2>0.99). Intra-day and 5 days repeatability showed an RSD

DOI:

Publication date: September 14, 2021

Issue: Macrowine 2021

Type: Article

Authors

Maurizio Piergiovanni

University of Trento, Centre Agriculture, Food, Environment (C3A), San Michele all’Adige, Italy,Silvia, CARLIN, Research and Innovation Centre, Food Quality and Nutrition Department, Fondazione Edmund Mach, San Michele all’Adige, Italy  Cesare, LOTTI, Research and Innovation Centre, Food Quality and Nutrition Department, Fondazione Edmund Mach, San Michele all’Adige, Italy.  Fulvio, MATTIVI, University of Trento, Centre Agriculture, Food, Environment (C3A), San Michele all’Adige, Italy.

Contact the author

Keywords

carbonyls, oxidation, ageing, accelerated ageing, solid-phase micro extraction, automatization, oxygen, off-flavors

Citation

Related articles…

A better understanding of the climate effect on anthocyanin accumulation in grapes using a machine learning approach

The current climate changes are directly threatening the balance of the vineyard at harvest time. The maturation period of the grapes is shifted to the middle of the summer, at a time when radiation and air temperature are at their maximum. In this context, the implementation of corrective practices becomes problematic. Unfortunately, our knowledge of the climate effect on the quality of different grape varieties remains very incomplete to guide these choices. During the Innovine project, original experiments were carried out on Syrah to study the combined effects of normal or high air temperature and varying degrees of exposure of the berries to the sun. Berries subjected to these different conditions were sampled and analyzed throughout the maturation period. Several quality characteristics were determined, including anthocyanin content. The objective of the experiments was to investigate which climatic determinants were most important for anthocyanin accumulation in the berries. Temperature and irradiance data, observed over time with a very thin discretization step, are called functional data in statistics. We developed the procedure SpiceFP (Sparse and Structured Procedure to Identify Combined Effects of Functional Predictors) to explain the variations of a scalar response variable (a grape berry quality variable for example) by two or three functional predictors (as temperature and irradiance) in a context of joint influence of these predictors. Particular attention was paid to the interpretability of the results. Analysis of the data using SpiceFP identified a negative impact of morning combinations of low irradiance (lower than about 100 μmol m−2 s−1 or 45 μmol m−2 s−1 depending on the advanced-delayed state of the berries) and high temperature (higher than 25oC). A slight difference associated with overnight temperature occurred between these effects identified in the morning.

Impact of geographical location on the phenolic profile of minority varieties grown in Spain. II: red grapevines

Because terroir and cultivar are drivers of wine quality, is essential to investigate theirs effects on polyphenolic profile before promoting the implantation of a red minority variety in a specific area. This work, included in MINORVIN project, focuses in the polyphenolic profile of 7 red grapevines minority varieties of Vitis vinifera L. (Morate, Sanguina, Santafe, Terriza Tinta Jeromo Tortozona Tinta) and Tempranillo) from six typical viticulture Spanish areas: Aragón (A1), Cataluña (A2), Castilla la Mancha (A3), Castilla –León (A4), Madrid (A5) and Navarra (A6) of 2020 season. Polyphenolic substances were extracted from grapes. 35 compounds were identified and quantified (mg subtance/kg fresh berry) by HPLC and grouped in anthocyanins (ANT) flavanols (FLAVA), flavonols (FLAVO), hydroxycinnamic (AH), benzoic (BA) acids and stilbenes (ST). Antioxidant activity (AA, mmol TE /g fresh berry) was determined by DPPH method. The results were submitted to a two-way ANOVA to investigate the influence of variety, area and their interaction for each polyphenolic family and cluster analysis was used to construct hierarchical dendrograms, searching the natural groupings among the samples. Sanguina (A3) had the most of total polyphenols while Tempranillo (A5) those of ANT. Sanguina (A2) and (A3) reached the highest values of FLAVO, FLAVA and AA. These two last samples had also the maximum of AA. The effect cultivar and area were significant for all polyphenolic families analyzed. A high variability due to variety (>50%) was observed in FLAVA and the maximum value of variability due to growing area was detected in AA (86.41%), ANT and FLAVO (51%); the interaction variety*zone was significant only for ANT, FLAVO, EST and AA. Finally, dendrograms presented five cluster: i) Sanguina (A2); ii) Sanguina (A3); iii) Tempranillo (A5); iv) Tempranillo (A3); Terriza (A3,A5), Morate (A5,A6); v) Santafé (A1,A6); Tortozona tinta (A1,A3,A6); Tinta Jeromo (A3,A4).

Late frost protection in Champagne

Probably one of the most counterintuitive impacts of climate change on vine is the increased frequency of late frost. Champagne, due to its septentrional position is historically and regularly affected by this meteorological hazard. Champagne has therefore developed a strong experience in frost protection with first experiments dating from the end of 19th century. Frost protection can be divided in two parts: passive and active. Passive protection includes all the methods that do not seek to modify the vine’s environment or resistance at the time of frost. The most iconic passive protection in Champagne is the establishment of the individual reserve. This reserve allows to stock a certain quantity of clear wine during a surplus year to compensate a meteorological hazard like frost during the following years. Other common passive methods are the control of planting area (walls, bushes, topography), the choice of grape variety, late pruning, or the impact of grass cover and tillage. Active frost protection is also divided in two parts. Most of the existing techniques tend to modify vine’s environment. Most of the time they provide warmth (candles, heaters, windmills, heating cables…), or stabilise bud’s temperature above a lethal threshold (water sprinkling). The other way to actively fight is to enhance the resistance of buds to frost (elicitors). The Comité Champagne evaluates frost protection methods following three main axes: the efficiency, the profitability, and the environmental impact through a lifecycle assessment. This study will present the results on both passive and active protection following these three axes.

Sustaining wine identity through intra-varietal diversification

With contemporary climate change, cultivated Vitis vinifera L. is at risk as climate is a critical component in defining ecologically fitted plant materiel. While winegrowers can draw on the rich diversity among grapevine varieties to limit expected impacts (Morales-Castilla et al., 2020), replacing a signature variety that has created a sense of local distinctiveness may lead to several challenges. In order to sustain wine identity in uncertain climate outcomes, the study of intra-varietal diversity is important to reflect the adaptive and evolutionary potential of current cultivated varieties. The aim of this ongoing study is to understand to what extent can intra-varietal diversity be a climate change adaptation solution. With a focus on early (Sauvignon blanc, Riesling, Grolleau, Pinot noir) to moderate late (Chenin, Petit Verdot, Cabernet franc) ripening varieties, data was collected for flowering and veraison for the various studied accessions (from conservatory plots) and clones. For these phenological growing stages, heat requirements were established using nearby weather stations (adapted from the GFV model, Parker et al., 2013) and model performances were verified. Climate change projections were then integrated to predict the future behaviour of the intra-varietal diversity. Study findings highlight the strong phenotypic diversity of studied varieties and the importance of diversification to enhance climate change resilience. While model performances may require improvements, this study is the first step towards quantifying heat requirements of different clones and how they can provide adaptation solutions for winegrowers to sustain local wine identity in a global changing climate. As genetic diversity is an ongoing process through point mutations and epigenetic adaptations, perspective work is to explore clonal data from a wide variety of geographic locations.

δ13C : A still underused indicator in precision viticulture  

The first demonstration of the interest of carbon isotope composition of sugars in grapevine, as an integrated indicator of vineyard water status, dates back to 2000 (Gaudillère et al., 1999; Van Leeuwen et al., 2001). Thanks to the isotopic discrimination of Carbon that takes place during plant photosynthesis, under hydric stress conditions, it is possible to accurately estimate the photosynthetic activity. Ever since, δ13C has been widely applied with success to zonation, terroir studies and vine physiology research, but is still not widely used by viticulturists. This is quite astonishing by considering the impact of global warming on viticulture and the need to improve water management, that would justify a widespread use of δ13C.
The lack of private laboratories proposing the analysis, the cost of the technology, as well as the long analytical delays, have been detrimental to its development. Some laboratories tried to overcome the analytical difficulties of isotopic analysis by using fourier transformed infrared spectroscopy, as a fast and cheap alternative to the official OIV method (IRMS). These claimed FTIR models have never been published or peer reviewed and cannot be considered robust. In this work, thanks to the recent acquisition of IRMS technology, new modern and robust applications of δ13C for viticulture are proposed. This includes the use of the analysis to make parcel separations at harvesting, the possibility to increase the precision of hydric stress cartography and the potential cost reduction when compared with Scholander pressure bomb analysis.