IVAS 2022 banner
IVES 9 IVES Conference Series 9 IVAS 9 IVAS 2022 9 Selective and sensitive quantification of wine biogenic amines using a dispersive solid-phase extraction clean-up/concentration method

Selective and sensitive quantification of wine biogenic amines using a dispersive solid-phase extraction clean-up/concentration method

Abstract

Biogenic amines exist in numerous foods, including wine. They can have aliphatic (putrescine, cadaverine, spermine, and spermidine), aromatic (tyramine and phenylethylamine) and heterocyclic structure (histamine and tryptamine). In wine, the biogenic amines have three possible origins, they can be present in the grape juice, can be formed during alcoholic fermentation by yeasts, or during malolactic fermentation by the action of lactic acid bacteria that can decarboxylate amino acids present in wine. Therefore, the main request for the formation of biogenic amines is the presence of free amino acids, the existence of decarboxylase-positive microorganisms, and environmental conditions that permit bacterial growth and decarboxylase synthesis and activity [1]. In low levels, biogenic amines contribute to physiological functions like regulation of stomach pH, body temperature, or brain activity. Nevertheless, the ingestion of wines comprising high levels of biogenic amines, numerous toxicological effects may happen for example headaches, nausea, and in severe situations intracerebral hemorrhage or even death [2].
Monitoring the existence of these compounds in wine is essential, not only from the toxicological perspective but also as an indicator of wine spoilage [3]. In this work, a simple dispersive solid-phase extraction (dSPE) was developed for sample clean-up and pre-concentration of biogenic amines in wine. The dSPE using a strong cation exchange resin increased the selectivity and sensitivity of the analysis by elimination of interfering compounds and a five-fold enrichment of biogenic amines. The derivatization with benzoyl chloride and then the extraction with diethyl ether steps were optimized. HPLC with diode array detector was used as an analytical technique and this method was validated for twelve biogenic amines – ethylamine, propylamine, butylamine, putrescine, cadaverin, typtamine, b-phenylethylamine, amylamine, spermidine, hexylamine, spermine, and histamine. The method presented an adequate precision and linearity with detection limits ranging from 0.133 to 0.509 mg/L. Recoveries ranging from 72 to 99% prove the accuracy of the method for determining biogenic amines in red, white, and Tawny Port wine samples yielding chromatograms clean from interferents [4]. The method was applied successfully to the analysis of 31 young commercial red wines from the 2016 vintage collected in wineries located in different Portuguese demarcated wine regions. The dSPE method developed is a simple, cheap, quick, and green sample clean-up strategy for biogenic amine analysis. Increasing their selective and sensitive UV detection, the more used detector in liquid chromatography. The results indicated that this method is suitable for the intended purpose with a good recovery, precision, detection, and quantification limits, and with a suitable range for the amounts of biogenic amines existing in wine. 

References

[1]R. E. Anli, M. Bayram, Food Reviews International, 25:1 (2008) 86-102.
[2] A. C. Manetta, L. D. Guiseppe, R., Tofalo, M. Martuscelli, M. Schirone, M. Giammarco, G. Suzzi. Food Control. 2016. 65, 351-356.
[3] L. Beneduce, A. Romano, V. Capozzi, P. Lucas, L. Barnavon, B. Bach, P. Vuchot, F. Grieco, G. Spano. Ann. Microbiol. 2010, 60, 573-578.
[4]J. Milheiro, L. C. Ferreira, L. Filipe-Ribeiro, F. Cosme, F. M. Nunes, Food Chemistry, 274 (2019) 110-117.

DOI:

Publication date: June 24, 2022

Issue: IVAS 2022

Type: Poster

Authors

Cosme Fernanda1, Milheiro Juliana1, Ferreira Leonor C.1, Filipe-Ribeiro Luís1 and Nunes Fernando M.1

1Chemistry Research Centre-Vila Real (CQ-VR), Food and Wine Chemistry Laboratory, University of Trás-os-Montes and Alto Douro, School of Life Sciences and Environment

Contact the author

Keywords

Red wine; Biogenic amines; Dispersive solid phase extraction; Derivatization, Histamine.

Tags

IVAS 2022 | IVES Conference Series

Citation

Related articles…

Delaying irrigation initiation linearly reduces yield with little impact on maturity in Pinot noir

When to initiate irrigation is a critical annual management decision that has cascading effects on grapevine productivity and wine quality in the context of climate change. A multi-site trial was begun in 2021 to optimize irrigation initiation timing using midday stem water potential (ψstem) thresholds characterized as departures from non-stressed baseline ψstemvalues (Δψstem). Plant material, vine and row spacing, and trellising systems were concomitant among sites, while vine age, soil type, and pruning systems varied. Five target Δψstem thresholds were arranged in an RCBD and replicated eight times at each site: 0.2, 0.4, 0.6, 0.8, and 1.0 MPa (T1, T2, T3, T4, and T5, respectively). When thresholds were reached, plots were irrigated weekly at 70% ETc. Yield components and berry composition were quantified at harvest. To better generalize inferences across sites, data were analyzed by ANOVA using a mixed model including site as a random factor. Across sites, irrigation was initiated at Δψstem = 0.24, 0.50, 0.65, 0.93, and 0.98 MPa for T1, T2, T3, T4, and T5, respectively. Consistent significant negative linear trends were found for several key yield and berry composition variables. Yield decreased by 12.9, 15.9, 19.5, and 27.4% for T2, T3, T4, and T5, respectively, compared to T1 (p < 0.0001) across sites that were driven by similarly linear reductions in berry weight (p < 0.0001). Comparatively, berry composition varied little among treatments. Juice total soluble solids decreased linearly from T1 to T5 – though only ranged 0.9 Brix (p = 0.012). Because producers are paid by the ton, and contracts simply stipulate a target maturity level, first-year results suggest that there is no economic incentive to induce moderate water deficits before irrigation initiation, regardless of vineyard site. Subsequent years will further elucidate the carryover effects of delaying irrigation initiation on productivity over the long term.

Aromatic maturity is a cornerstone of terroir expression in red wine

Harvesting grapes at adequate maturity is key to the production of high-quality red wines. Enologists and wine makers define several types of maturity, including technical maturity, phenolic maturity and aromatic maturity. Technical maturity and phenolic maturity are relatively well documented in the scientific literature, while articles on aromatic maturity are scarcer. This is surprising, because aromatic maturity is, without a doubt, the most important of the three in determining wine quality and typicity (including terroir expression). Optimal terroir expression can be obtained when the different types of maturity are reached at the same time, or within a short time frame. This is more likely to occur when the ripening takes place under mild temperatures, neither too cool, nor too hot. Aromatic expression in wine can be driven, from low to high maturity, by green, herbal, fresh fruit, ripe fruit, jammy fruit, candied fruit or cooked fruit aromas. Green and cooked fruit aromas are not desirable in red wines, while the levels of other aromatic compounds contribute to the typicity of the wine in relation to its origin. Wines produced in cool climates, or on cool soils in temperate climates, are likely to express herbal or fresh fruit aromas; while wines produced under warm climates, or on warm soils in temperate climates, may express ripe fruit, jammy fruit or candied fruit aromas. Growers can optimize terroir expression through their choice of grapevine variety. Early ripening varieties perform better in cool climates and late ripening varieties in warm climates. Additionally, maturity can be advanced or delayed by different canopy management practices or training systems.

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.

Modeling the suitability of Pinot Noir in Oregon’s Willamette Valley in a changing climate

Air temperature is the key driver of grapevine phenology and a significant environmental factor impacting yield and quality for a winegrape growing region. In this study the optimal downscaled CMIP5 ensemble for computing thegrowing season average temperature (GST) viticulture climate classification index was determined to spatially compute on a decadal basis predictions of the GST climate index and the grapevine sugar ripeness (GSR) model for Pinot Noir throughout the Willamette Valley (WV) American Viticultural Area (AVA). Forecasts for average temperature and a 220 g/L target sugar concentration level were computed using daily Localized Constructed Analogs (LOCA) downscaled CMIP5 historic and Representative Concentration Pathways (RCP) future climate projections of minimum and maximum daily temperature. We explore spatiotemporal trends of the GST climate classification index and Pinot Noir specific applications of the GSR phenology model for the WV AVA. Spatiotemporal computations of the GST climate index and Pinot Noir specific applications of the GSR model enable the opportunity to explore relationships between their computed values with one intent being to provide updated GST ranges that better align with current temperature-based modeling understanding of Pinot Noir grapevine phenology and the viticultural application of LOCA CMIP5 climate projections for the WV AVA. The Pinot Noir specific applications of the GSR model or the GST index with updated bounds indicate that the percent of the WV AVA area suitable for Pinot Noir production is currently at or near its peak value in the upper 80s to lower 90s of this century.

VINIoT – Precision viticulture service

The project VINIoT pursues the creation of a new technological vineyard monitoring service, which will allow companies in the wine sector in the SUDOE space to monitor plantations in real time and remotely at various levels of precision. The system is based on spectral images and an IoT architecture that allows assessing parameters of interest viticulture and the collection of data at a precise scale (level of grape, plant, plot or vineyard) will be designed. In France, three subjects were specifically developed: evaluation of maturity, of water stress, and detection of flavescence dorée. For the evaluation of maturity, it has been decided first to work at the berry scale in the laboratory, then at the bunch scale and finally in the vineyard. The acquisition of the spectral hyperstal image as well as the reference analyzes to measure the maturity, were carried out in the laboratory after harvesting the berries in a maturity monitoring context. This work focuses on a case study to predict sugar content of three different grape varieties: Syrah, Fer Servadou and Mauzac. A robust method called Roboost-PLSR, developed in the framework of this work (Courand et al., 2022), to improve prediction model performance was applied on spectra after the acquirement of hyperspectral images. Regarding the evaluation of water stress, to work with a significant variability in terms of water status, it has been worked first with potted plants under 2 different water regimes. The facilities have allowed the supervision of irrigation and micro-climatic conditions. The regression models on agronomic variables (stomatal conductance, water potential, …) are studied. To detect flavescence dorée, the experimental plan has consisted of work at leaf scale in the laboratory first, and then in the field. To detect the disease from hyper-spectral imaging, a combination of multivariate curve resolution-alternating least squares (MCR-ALS) and factorial discriminant analysis (FDA) was proposed. This strategy proved the potential towards the discrimination of healthy and infected leaves by flavescence dorée based on the use of hyperspectral images (Mas Garcia et al., 2021).