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…

Vineyards and clay minerals: multi-technique analytical approach and correlations with soil properties

Purpose of this research is to quantitatively assess the mineral component of vineyard soils, with particular attention to the mineralogical analysis of clays, which represent an element of high importance in the vineyard culture as well as in general agriculture. An X-ray diffraction (XRD) / thermogravimetric (TG) multi-technique analytical approach was developed, tested on soil samples taken from vineyards around the world. This codified analytical procedure was necessary to obtain precise qualitative and quantitative mineralogical data, globally comparable to distinguish the geopedological identity of the vineyards. Soil samples from vineyards of various locations were analysed, in very different geological conditions. The bulk-rock quantitative phase analysis (QPA) was obtained by the Rietveld method while the detailed composition of the clay-sized fraction was determined by modelling of the oriented X-ray diffraction patterns. The research provided a precise classification of the mineral component of soils, distinguishing the mineral phases of the clays and the so-called mixed-layer clay minerals. We found that the content in mixed layers can be directly correlated with the water retention and the cation exchange capacity ​​of the soil, while the presence of other clayey minerals and phyllosilicates in this research did not affect this CEC parameter, which codes the fertility level of the soils. The study demonstrates that terroir, in particular soils formed in complex or very different geological conditions, can only be effectively interpreted by properly analysing its mineral phases, in particular the mixed-layer clay component. These are characteristic abiotic ecological indicators, which may have specific eco-physiological influences on the plant.

Use of a new, miniaturized, low-cost spectral sensor to estimate and map the vineyard water status from a mobile 

Optimizing the use of water and improving irrigation strategies has become increasingly important in most winegrowing countries due to the consequences of climate change, which are leading to more frequent droughts, heat waves, or alteration of precipitation patterns. Optimized irrigation scheduling can only be based on a reliable knowledge of the vineyard water status.

In this context, this work aims at the development of a novel methodology, using a contactless, miniaturized, low-cost NIR spectral tool to monitor (on-the-go) the vineyard water status variability. On-the-go spectral measurements were acquired in the vineyard using a NIR micro spectrometer, operating in the 900–1900 nm spectral range, from a ground vehicle moving at 3 km/h. Spectral measurements were collected on the northeast side of the canopy across four different dates (July 8th, 14th, 21st and August 12th) during 2021 season in a commercial vineyard (3 ha). Grapevines of Vitis vinifera L. Graciano planted on a VSP trellis were monitored at solar noon using stem water potential (Ψs) as reference indicators of plant water status. In total, 108 measurements of Ψs were taken (27 vines per date).

Calibration and prediction models were performed using Partial Least Squares (PLS) regression. The best prediction models for grapevine water status yielded a determination coefficient of cross-validation (r2cv) of 0.67 and a root mean square error of cross-validation (RMSEcv) of 0.131 MPa. This predictive model was employed to map the spatial variability of the vineyard water status and provided useful, practical information towards the implementation of appropriate irrigation strategies. The outcomes presented in this work show the great potential of this low-cost methodology to assess the vineyard stem water potential and its spatial variability in a commercial vineyard.

Exploring resilience and competitiveness of wine estates in Languedoc-Roussillon in the recent past: a multi-level perspective

The Languedoc-Roussillon wineries are facing a decline in wine yields particularly PGI yields due to many factors. Climate change is just ones, but is expected to increase in the future. There is also structurally a large heterogeneity of yield profiles among terroirs, varieties and strategies. This work investigates the link between yield, competitiveness and resilience to explore how resilient winegrowers have been in the recent past. To this end two approaches have been combined; (i) an accountancy database analysis at estate scale and (ii) municipality level competitiveness analysis. A new resilience indicator that characterizes the capacity of an estate to absorb yield variation is also defined. The FADN database between 2000 and 2018 of ex-Languedoc-Roussillon (France) and other data are used to analyse the current situation and the past evolution of competitiveness and resilience by type of estate (type of farm: PGI and/or PDO & type of commercialization: bulk and/or bottles). The net margin, which defines competitiveness, is not correlated to yield for all types but depends on the type of commercialization and the level of specialisation. The resilience indicator shows that the net margin of estates specialized in PGI is particularly sensitive to yield declines. We also show that price evolutions seem to compensate the effect of yield losses for the majority of types. Municipality scale analysis shows the links between local pedoclimate, yield, commercialization strategies and price. Overlapping a PDO with a PGI does not always increase a municipality’s PGI competitiveness. It is difficult to make links between causes and effects due to the complexity of the wine production system. Production diversification may be a solution. Resorting to the two level of analysis helps resolving the data gap that is necessary to explore the links between yield and economic performance of the wine estates in the long term.

Use of multispectral satellite for monitoring vine water status in mediterranean areas

The development of new generations of multispectral satellites such as Sentinel-2 opens possibilities as to vine water status assessment (Cohen et al., 2019). Based on a three years field campaign, a model of Stem Water Potential (SWP) estimation on vine using four satellite bands in Red, Red-Edge, NIR and SWIR domains was developed (Laroche-Pinel et al., 2021). The model relies on SWP field measures done using a pressure chamber (Scholander et al., 1965), which is a common, robust and precise method to assess vine water status (Acevedo-Opazo et al., 2008). The model was mainly developed from from SWP measures on Syrah N (Laroche Pinel E., 2021).

A large scale monitoring was organized in different vineyards in the Mediterranean region in 2021. 10 varieties amongst the most represented in this area were monitored (Cabernet sauvignon N, Chardonnay B, Cinsault N, Grenache N, Merlot N, Mourvèdre N, Sauvignon B, Syrah N, Vermentino B, Viognier B). The model was used to produce water status maps from Sentinel-2 images, starting from the beginning of June (fruit set) up to September (harvest). The average estimated SWP for each vine was compared to actual field SWP measures done by wine growers or technicians during usual monitoring of irrigation programs. The correlations between mean estimated SWP and mean measured SWP were at the same level than expected by the model. (Laroche Pinel, 2021) The general SWP kinetics were comparable. The estimated SWP would have led to same irrigation decisions concerning the date of first irrigation in comparison with measured SWP.

Acevedo-Opazo, C., Tisseyre, B., Ojeda, H., Ortega-Farias, S., Guillaume, S. (2008). Is it possible to assess the spatial variability of vine water status? OENO One, 42(4), 203.
Cohen, Y., Gogumalla, P., Bahat, I., Netzer, Y., Ben-Gal, A., Lenski, I., … Helman, D. (2019). Can time series of multispectral satellite images be used to estimate stem water potential in vineyards? In Precision agriculture ’19, The Netherlands: Wageningen Academic Publishers, pp. 445–451.
Laroche-Pinel, E., Duthoit, S., Albughdadi, M., Costard, A. D., Rousseau, J., Chéret, V., & Clenet, H. (2021). Towards vine water status monitoring on a large scale using sentinel-2 images. remote sensing, 13(9), 1837.
Laroche-Pinel,E. (2021). Suivi du statut hydrique de la vigne par télédétection hyper et multispectrale. Thèse INP Toulouse, France.
Scholander, P.F., Bradstreet, E.D., Hemmingsen, E.A., & Hammel, H.T. (1965). Sap pressure in vascular plants: Negative hydrostatic pressure can be measured in plants. Science, 148(3668), 339–346.

Influence of a spontaneous cover crop on the vineyard and soil erosion under Mediterranean climate

Sixty five % of the agricultural area of the Basque Country located in the DO Ca Rioja corresponds to vineyards. More than 40% of it has an average slope greater than 10%, which makes it sensitive to erosive processes. Furthermore, it is foreseeable that extreme weather events (storms, hail, extreme heat and cold, etc.) will be favored due to climate change. Cover cropping can mitigate this risk, and therefore the objective of this work is to evaluate the impact that a vegetable cover has on the agronomic behavior of the vineyard, the quality of the grape and soil erosion. For this, a trial has been carried out with a Graciano variety vineyard with a slope between 10% -20% during the years 2020 and 2021. Conventional tillage management in the area has been compared (4-6 passes per year of tillage machinery) versus spontaneous vegetation cover management in the vineyard. This implies not tilling and allowing the grass of the land to colonize the range between the lines of vines, controlling their height through 1-3 mowing passes per year, always trying to affect the surface of the land as little as possible. The vegetative growth, yield and quality of the grape and wine was measured. Furthermore, erosion has been measured using Gerlasch boxes. The yield was lower in the second year of the trial in the cover crop treatment, but erosion was significantly reduced.