IVAS 2022 banner
IVES 9 IVES Conference Series 9 IVAS 9 IVAS 2022 9 Study of the grape glycosidic aroma precursors by crossing SPE-GC/MS, SPME-GC/MS and LC/QTOF methods

Study of the grape glycosidic aroma precursors by crossing SPE-GC/MS, SPME-GC/MS and LC/QTOF methods

Abstract

Depending on the variety, grapes contain several chemical classes of aromatic compounds (i.e., terpenols, norisoprenoids, benzenoids) mainly stored as glycosides in berry skin. These secondary metabolites are the aromatic precursors fraction of grape which is liberated in wine during fermentation. Knowledge of their profile is often required to estimate the aromatic potential transferable to the wine and for chemotaxonomic aims (Nasi et al., 2008; Ferreira and Lopez, 2019).

In general, the methods used to study glycosidic aroma profile involve sample extraction and concentration by passage of large volumes of must or grape extract through a SPE cartridge (the stationary phases commonly used are 1-10 g of C18 or polystyrene-divinylbenzene), then the methanolic fraction eluted containing the glycoside compounds is carried to dryness, resolubilized using a citrate pH 5 buffer, and an enzymatic hydrolysis is carried out overnight to liberate the aglycones which are then analyzed by GC/MS. Main advantage of SPE is until 1000-fold concentration of sample which allows to detect also compounds present at low level but which can play important role in determining the organoleptic characteristics of wine. Usually, the selectivity of SPE towards the compounds studied is low, so performing quantitation by expressing the compounds as mg internal standard/kg grape provides accuracy acceptable for the aim of the study. On the other hand, SPE is laborious, needs long time and is hardly applicable in quality control laboratories. SPME is faster but the selectivity of fiber towards the analytes is often very different and to perform acceptable quantitative analysis it is essential the calculation of calibration curves. Unfortunately, just few standards of the grape aroma compounds are commercially available (Panighel et al., 2014).

In this study SPE-GC/MS and SPME-GC/MS methods are compared by performing analysis of a set of model standard solutions and grape must samples. The use of several internal standards allows to estimate recoveries of the analytes and calculation of corrective coefficients between the two methods. To have also information free of enzymatic artifacts, GC/MS results are crossed with profile of glycosidic aroma precursors determined by LC/QTOF analysis (Flamini et al., 2014).

The study is finalized to develop a quick SPME-GC/MS method which provides exhaustive and reliable qualitative and semi-quantitative information on the grape glycosidic aroma precursors

References

Nasi A., Ferranti P., Amato S., Chianese L. (2008). Food Chem. 110: 762-768
Ferreira V., Lopez R. (2019). Biomolecules 9(12): 818- doi:10.3390/biom9120818
Panighel A., Flamini R. (2014). Molecules 19: 21291-21309 doi:10.3390/molecules191221291
Flamini R., De Rosso M., Panighel A., Dalla Vedova A., De Marchi F., Bavaresco L. (2014). J. Mass Spec. 49(12): 1214-1222 doi:10.1002/jms.34411214

DOI:

Publication date: June 23, 2022

Issue: IVAS 2022

Type: Article

Authors

Panighel Annarita¹, Fugaro Michele², Mazzei Raffaele Antonio², De Rosso Mirko¹, De Marchi Fabiola¹ and Flamini Riccardo¹

¹Council for Agricultural Research and Economics – Viticulture & Oenology (CREA-VE)
²Dipartimento dell’Ispettorato centrale della tutela della qualità e repressione frodi dei prodotti agroalimentari – ICQRF NORD-EST

Contact the author

Keywords

Glycosides, grape, aroma, mass spectrometry

Tags

IVAS 2022 | IVES Conference Series

Citation

Related articles…

The potential of multispectral/hyperspectral technologies for early detection of “flavescence dorée” in a Portuguese vineyard

“Flavescence dorée” (FD) is a grapevine quarantine disease associated with phytoplasmas and transmitted to healthy plants by insect vectors, mainly Scaphoideus titanus. Infected plants usually develop symptoms of stunted growth, unripe cane wood, leaf rolling, leaf yellowing or reddening, and shrivelled berries. Since plants can remain symptomless up to four years, they may act as reservoirs of FD contributing to the spread of the disease. So far, conventional management strategies rely mainly on the insecticide treatments, uprooting of infected plants and use of phytoplasma-free propagation material. However, these strategies are costly and could have undesirable environmental impacts. Thus, the development of sustainable and noninvasive approaches for early detection of FD and its management are of great importance to reduce disease spread and select the best cultural practices and treatments. The present study aimed to evaluate if multispectral/hyperspectral technologies can be used to detect FD before the appearance of the first symptoms and if infected grapevines display a spectral imaging fingerprint. To that end, physiological parameters (leaf area, chlorophyll content and photosynthetic rate) were collected in concomitance to the measurements of plant reflectance (using both a portable apparatus and a remote sensing drone). Measurements were performed in two leaves of 8 healthy and 8 FD-infected grapevines, at four timepoints: before the development of disease symptoms (21st June); and after symptoms appearance (ii) at veraison (2nd August); at post-veraison (11th September); and at harvest (25th September). At all timepoints, FD infected plants revealed a significant decrease in the studied physiological parameters, with a positive correlation with drone imaging data and portable apparatus analyses. Moreover, spectra of either drone imaging and portable apparatus showed clear differences between healthy and FD-infected grapevines, validating multispectral/ hyperspectral technology as a potential tool for the early detection of FD or other grapevine-associated diseases.

Teasing apart terroir: the influence of management style on native yeast communities within Oregon wineries and vineyards

Newer sequencing technologies have allowed for the addition of microbes to the story of terroir. The same environmental factors that influence the phenotypic expression of a crop also shape the composition of the microbial communities found on that crop. For fermented goods, such as wine, that microbial community ultimately influences the organoleptic properties of the final product that is delivered to customers. Recent studies have begun to study the biogeography of wine-associated microbes within different growing regions, finding that communities are distinct across landscapes. Despite this new knowledge, there are still many questions about what factors drive these differences. Our goal was to quantify differences in yeast communities due to management style between seven pairs of conventional and biodynamic vineyards (14 in total) throughout Oregon, USA. We wanted to answer the following questions: 1) are yeast communities distinct between biodynamic vineyards and conventional vineyards? 2) are these differences consistent across a large geographic region? 3) can differences in yeast communities be tied to differences in metabolite profiles of the bottled wine? To collect our data we took soil, bark, leaf, and grape samples from within each vineyard from five different vines of pinot noir. We also collected must and a 10º brix sample from each winery. Using these samples, we performed 18S amplicon sequencing to identify the yeast present. We then used metabolomics to characterize the organoleptic compounds present in the bottled wine from the blocks the year that we sampled. We are actively in the process of analysing our data from this study.

Terroir analysis and its complexity

Terroir is not only a geographical site, but it is a more complex concept able to express the “collective knowledge of the interactions” between the environment and the vines mediated through human action and “providing distinctive characteristics” to the final product (OIV 2010). It is often treated and accepted as a “black box”, in which the relationships between wine and its origin have not been clearly explained. Nevertheless, it is well known that terroir expression is strongly dependent on the physical environment, and in particular on the interaction between soil-plant and atmosphere system, which influences the grapevine responses, grapes composition and wine quality. The Terroir studying and mapping are based on viticultural zoning procedures, obtained with different levels of know-how, at different spatial and temporal scales, empiricism and complexity in the description of involved bio-physical processes, and integrating or not the multidisciplinary nature of the terroir. The scientific understanding of the mechanisms ruling both the vineyard variability and the quality of grapes is one of the most important scientific focuses of terroir research. In fact, this know-how is crucial for supporting the analysis of climate change impacts on terroir resilience, identifying new promised lands for viticulture, and driving vineyard management toward a target oenological goal. In this contribution, an overview of the last findings in terroir studies and approaches will be shown with special attention to the terroir resilience analysis to climate change, facing the use and abuse of terroir concept and new technology able to support it and identifying the terroir zones.

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.

Climate, Viticulture, and Wine … my how things have changed!

The planet is warmer than at any time in our recorded past and increasing greenhouse emissions and persistence in the climate system means that continued warming is highly likely. Climate change has already altered the basic framework of growing grapes for wine production worldwide and will likely continue to do so for years to come. The wine sector can continue to play an important role in leading the agricultural sector in addressing climate change. From developing on…