Optimization and Validation of a Method to Determine Enolones and Vanillin Derivatives in Wines—Occurrence in Spanish Red Wines and Mistelles

Understanding the chemical nature of wine aroma demands accurate quantitative determinations of different odor-active compounds. Quantitative determinations of enolones (maltol, furaneol, homofuraneol, and sotolon) and vanillin derivatives (vanillin, methyl vanillate, ethyl vanillate, and acetovanillone) at low concentrations are complicated due to their high polarity. For this reason, this paper presents an improved and automated version for the accurate measure of these common trace wine polar compounds (enolones and vanillin derivatives). As a result, a faster and more user-friendly method with a reduction of organic solvents and resins was developed and validated. The optimization of some stages of the solid phase extraction (SPE) process, such as washing with an aqueous solution containing 1% NaHCO at pH 8, led to cleaner extracts and solved interference problems. Due to the polarity of these type of compounds, an optimization of the large volume injection was also carried out. Finally, a programmable temperature vaporization (PTV) quartz glass inlet liner without wool was used. The injector temperature was raised to 300 °C in addition to applying a pressure pulse of 180 kPa for 4 min. Matrix effects were solved by the use of adequate internal standards, such as ethyl maltol and 3′,4′-(methylenedioxy)acetophenone. Method figures of merit were highly satisfactory: good linearity (r > 0.98), precision (relative standard deviation, RSD < 10%), high recovery (RSD > 89%), and low detection limits (<0.7 μg/L). Enolones and vanillin derivatives are associated with wine aging. For this reason, the methodology was successfully applied to the quantification of these compounds in 16 Spanish red wines and 12 mistelles. Odor activity values (OAV) indicate that furaneol should be considered an aroma impact odorant in red wines and mistelles (OAV > 1) while homofuraneol and sotolon could also produce changes in their aroma perceptions (0.1 < OAV < 1).

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Main Authors: Bueno, Mónica, Zapata, Julián, Culleré, Laura, Franco-Luesma, Ernesto, De-La-Fuente-Blanco, Arancha, Ferreira, Vicente
Other Authors: Agencia Estatal de Investigación (España)
Format: artículo biblioteca
Published: Molecular Diversity Preservation International 2023
Subjects:Polar metabolites, Enolones, Vanillin derivatives, Sotolon, Furaneol, Vanillin, Wine, Mistelle, Odor activity value,
Online Access:http://hdl.handle.net/10261/337315
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spelling dig-icvv-es-10261-3373152023-10-18T08:53:59Z Optimization and Validation of a Method to Determine Enolones and Vanillin Derivatives in Wines—Occurrence in Spanish Red Wines and Mistelles Bueno, Mónica Zapata, Julián Culleré, Laura Franco-Luesma, Ernesto De-La-Fuente-Blanco, Arancha Ferreira, Vicente Agencia Estatal de Investigación (España) Ministerio de Ciencia e Innovación (España) Gobierno de Aragón European Commission Ministerio de Ciencia, Innovación y Universidades (España) Polar metabolites Enolones Vanillin derivatives Sotolon Furaneol Vanillin Wine Mistelle Odor activity value Understanding the chemical nature of wine aroma demands accurate quantitative determinations of different odor-active compounds. Quantitative determinations of enolones (maltol, furaneol, homofuraneol, and sotolon) and vanillin derivatives (vanillin, methyl vanillate, ethyl vanillate, and acetovanillone) at low concentrations are complicated due to their high polarity. For this reason, this paper presents an improved and automated version for the accurate measure of these common trace wine polar compounds (enolones and vanillin derivatives). As a result, a faster and more user-friendly method with a reduction of organic solvents and resins was developed and validated. The optimization of some stages of the solid phase extraction (SPE) process, such as washing with an aqueous solution containing 1% NaHCO at pH 8, led to cleaner extracts and solved interference problems. Due to the polarity of these type of compounds, an optimization of the large volume injection was also carried out. Finally, a programmable temperature vaporization (PTV) quartz glass inlet liner without wool was used. The injector temperature was raised to 300 °C in addition to applying a pressure pulse of 180 kPa for 4 min. Matrix effects were solved by the use of adequate internal standards, such as ethyl maltol and 3′,4′-(methylenedioxy)acetophenone. Method figures of merit were highly satisfactory: good linearity (r > 0.98), precision (relative standard deviation, RSD < 10%), high recovery (RSD > 89%), and low detection limits (<0.7 μg/L). Enolones and vanillin derivatives are associated with wine aging. For this reason, the methodology was successfully applied to the quantification of these compounds in 16 Spanish red wines and 12 mistelles. Odor activity values (OAV) indicate that furaneol should be considered an aroma impact odorant in red wines and mistelles (OAV > 1) while homofuraneol and sotolon could also produce changes in their aroma perceptions (0.1 < OAV < 1). Funded by the Spanish Ministry of Science and Innovation (MICINN) (project PID2021-126031OB-C2). LAAE acknowledges the continuous support of Gobierno de Aragón (T29) and European Social Fund. M.B. would like to acknowledge the Spanish National Research Agency (AEI) and the Ministry of Science, Innovation, and Universities (MICIU) for her “Juan de la Cierva-Incorporación” postdoctoral grant IJC2018-037830-I. 2023-10-18T08:50:04Z 2023-10-18T08:50:04Z 2023 2023-10-18T08:50:04Z artículo doi: 10.3390/molecules28104228 e-issn: 1420-3049 Molecules 28(10): 4228 (2023) http://hdl.handle.net/10261/337315 #PLACEHOLDER_PARENT_METADATA_VALUE# #PLACEHOLDER_PARENT_METADATA_VALUE# info:eu-repo/grantAgreement/AEI//PID2021-126031OB-C2 info:eu-repo/grantAgreement/AEI//IJC2018-037830-I Publisher's version The underlying dataset has been published as supplementary material of the article in the publisher platform at http://dx.doi.org/10.3390/molecules28104228 http://dx.doi.org/10.3390/molecules28104228 Sí open application/pdf Molecular Diversity Preservation International
institution ICVV ES
collection DSpace
country España
countrycode ES
component Bibliográfico
access En linea
databasecode dig-icvv-es
tag biblioteca
region Europa del Sur
libraryname Biblioteca del ICVV España
topic Polar metabolites
Enolones
Vanillin derivatives
Sotolon
Furaneol
Vanillin
Wine
Mistelle
Odor activity value
Polar metabolites
Enolones
Vanillin derivatives
Sotolon
Furaneol
Vanillin
Wine
Mistelle
Odor activity value
spellingShingle Polar metabolites
Enolones
Vanillin derivatives
Sotolon
Furaneol
Vanillin
Wine
Mistelle
Odor activity value
Polar metabolites
Enolones
Vanillin derivatives
Sotolon
Furaneol
Vanillin
Wine
Mistelle
Odor activity value
Bueno, Mónica
Zapata, Julián
Culleré, Laura
Franco-Luesma, Ernesto
De-La-Fuente-Blanco, Arancha
Ferreira, Vicente
Optimization and Validation of a Method to Determine Enolones and Vanillin Derivatives in Wines—Occurrence in Spanish Red Wines and Mistelles
description Understanding the chemical nature of wine aroma demands accurate quantitative determinations of different odor-active compounds. Quantitative determinations of enolones (maltol, furaneol, homofuraneol, and sotolon) and vanillin derivatives (vanillin, methyl vanillate, ethyl vanillate, and acetovanillone) at low concentrations are complicated due to their high polarity. For this reason, this paper presents an improved and automated version for the accurate measure of these common trace wine polar compounds (enolones and vanillin derivatives). As a result, a faster and more user-friendly method with a reduction of organic solvents and resins was developed and validated. The optimization of some stages of the solid phase extraction (SPE) process, such as washing with an aqueous solution containing 1% NaHCO at pH 8, led to cleaner extracts and solved interference problems. Due to the polarity of these type of compounds, an optimization of the large volume injection was also carried out. Finally, a programmable temperature vaporization (PTV) quartz glass inlet liner without wool was used. The injector temperature was raised to 300 °C in addition to applying a pressure pulse of 180 kPa for 4 min. Matrix effects were solved by the use of adequate internal standards, such as ethyl maltol and 3′,4′-(methylenedioxy)acetophenone. Method figures of merit were highly satisfactory: good linearity (r > 0.98), precision (relative standard deviation, RSD < 10%), high recovery (RSD > 89%), and low detection limits (<0.7 μg/L). Enolones and vanillin derivatives are associated with wine aging. For this reason, the methodology was successfully applied to the quantification of these compounds in 16 Spanish red wines and 12 mistelles. Odor activity values (OAV) indicate that furaneol should be considered an aroma impact odorant in red wines and mistelles (OAV > 1) while homofuraneol and sotolon could also produce changes in their aroma perceptions (0.1 < OAV < 1).
author2 Agencia Estatal de Investigación (España)
author_facet Agencia Estatal de Investigación (España)
Bueno, Mónica
Zapata, Julián
Culleré, Laura
Franco-Luesma, Ernesto
De-La-Fuente-Blanco, Arancha
Ferreira, Vicente
format artículo
topic_facet Polar metabolites
Enolones
Vanillin derivatives
Sotolon
Furaneol
Vanillin
Wine
Mistelle
Odor activity value
author Bueno, Mónica
Zapata, Julián
Culleré, Laura
Franco-Luesma, Ernesto
De-La-Fuente-Blanco, Arancha
Ferreira, Vicente
author_sort Bueno, Mónica
title Optimization and Validation of a Method to Determine Enolones and Vanillin Derivatives in Wines—Occurrence in Spanish Red Wines and Mistelles
title_short Optimization and Validation of a Method to Determine Enolones and Vanillin Derivatives in Wines—Occurrence in Spanish Red Wines and Mistelles
title_full Optimization and Validation of a Method to Determine Enolones and Vanillin Derivatives in Wines—Occurrence in Spanish Red Wines and Mistelles
title_fullStr Optimization and Validation of a Method to Determine Enolones and Vanillin Derivatives in Wines—Occurrence in Spanish Red Wines and Mistelles
title_full_unstemmed Optimization and Validation of a Method to Determine Enolones and Vanillin Derivatives in Wines—Occurrence in Spanish Red Wines and Mistelles
title_sort optimization and validation of a method to determine enolones and vanillin derivatives in wines—occurrence in spanish red wines and mistelles
publisher Molecular Diversity Preservation International
publishDate 2023
url http://hdl.handle.net/10261/337315
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