Quantitative determination of wine polyfunctional mercaptans at nanogram per liter level by gas chromatography–negative ion mass spectrometric analysis of their pentafluorobenzyl derivatives

A fast method for the determination of aroma-powerful polyfunctional thiols at nanogram per liter level has been developed and applied to wine. A small volume of wine (6 mL) was extracted with 1.5 mL of benzene containing four internal standards. Pentafluorobenzyl derivatives of mercaptans were form...

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Detalhes bibliográficos
Autores: Mateo Vivaracho, Laura María, Cacho, Juan, Ferreira, Vicente
Formato: artículo
Estado:Versión publicada
Fecha de publicación:2007
País:España
Recursos:Universidad de Valladolid
Repositorio:UVaDOC. Repositorio Documental de la Universidad de Valladolid
OAI Identifier:oai:uvadoc.uva.es:10324/73732
Acesso em linha:https://doi.org/10.1016/j.chroma.2007.02.003
https://uvadoc.uva.es/handle/10324/73732
Access Level:acceso abierto
Palavra-chave:Thiols
Pentafluorobenzylbromide
GC–NCI–MS
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spelling Quantitative determination of wine polyfunctional mercaptans at nanogram per liter level by gas chromatography–negative ion mass spectrometric analysis of their pentafluorobenzyl derivativesMateo Vivaracho, Laura MaríaCacho, JuanFerreira, VicenteThiolsPentafluorobenzylbromideGC–NCI–MSA fast method for the determination of aroma-powerful polyfunctional thiols at nanogram per liter level has been developed and applied to wine. A small volume of wine (6 mL) was extracted with 1.5 mL of benzene containing four internal standards. Pentafluorobenzyl derivatives of mercaptans were formed in the extract by adding small amounts (100 mg L−1) of pentafluorobenzyl bromide and a strong alkali: 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU). After washing with a water:methanol (5:1) solution 0.5 M in HCl, 20 L of the extract was directly injected into a gas chromatograph. Derivatives were detected by negative ion mass spectrometry. The method makes it possible to simultaneously determine 2-furfurylthiol (2-furanmethanethiol) (FFT), 4-mercapto-4-methyl-2-pentanone (MP), 3-mercaptohexylacetate (MHA) and 3-mercaptohexanol (MH). Inconsistent results were obtained for 2-methyl-3-furanthiol (MF). Detection limits were 0.5 ng L−1 (FFT), 0.1 ng L−1 (MP), 0.6 ng L−1 (MHA) and 7 ng L−1 (MH), well below the corresponding odor detection thresholds. Method repeatability (10% < RSD < 17%) and linearity (0.98 < R2 < 0.999) were satisfactory. The linear range was more than 2 orders of magnitude wide, covering the natural range of occurrence of these compounds in wine, and the slopes of the standard addition plots from different wines were very similar. The different aspects of the method optimization are discussed.Elsevier2007info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionapplication/pdfhttps://doi.org/10.1016/j.chroma.2007.02.003https://uvadoc.uva.es/handle/10324/73732reponame:UVaDOC. Repositorio Documental de la Universidad de Valladolidinstname:Universidad de ValladolidInglésinfo:eu-repo/semantics/openAccesshttp://creativecommons.org/licenses/by-nc-nd/4.0/oai:uvadoc.uva.es:10324/737322026-06-13T12:44:47Z
dc.title.none.fl_str_mv Quantitative determination of wine polyfunctional mercaptans at nanogram per liter level by gas chromatography–negative ion mass spectrometric analysis of their pentafluorobenzyl derivatives
title Quantitative determination of wine polyfunctional mercaptans at nanogram per liter level by gas chromatography–negative ion mass spectrometric analysis of their pentafluorobenzyl derivatives
spellingShingle Quantitative determination of wine polyfunctional mercaptans at nanogram per liter level by gas chromatography–negative ion mass spectrometric analysis of their pentafluorobenzyl derivatives
Mateo Vivaracho, Laura María
Thiols
Pentafluorobenzylbromide
GC–NCI–MS
title_short Quantitative determination of wine polyfunctional mercaptans at nanogram per liter level by gas chromatography–negative ion mass spectrometric analysis of their pentafluorobenzyl derivatives
title_full Quantitative determination of wine polyfunctional mercaptans at nanogram per liter level by gas chromatography–negative ion mass spectrometric analysis of their pentafluorobenzyl derivatives
title_fullStr Quantitative determination of wine polyfunctional mercaptans at nanogram per liter level by gas chromatography–negative ion mass spectrometric analysis of their pentafluorobenzyl derivatives
title_full_unstemmed Quantitative determination of wine polyfunctional mercaptans at nanogram per liter level by gas chromatography–negative ion mass spectrometric analysis of their pentafluorobenzyl derivatives
title_sort Quantitative determination of wine polyfunctional mercaptans at nanogram per liter level by gas chromatography–negative ion mass spectrometric analysis of their pentafluorobenzyl derivatives
dc.creator.none.fl_str_mv Mateo Vivaracho, Laura María
Cacho, Juan
Ferreira, Vicente
author Mateo Vivaracho, Laura María
author_facet Mateo Vivaracho, Laura María
Cacho, Juan
Ferreira, Vicente
author_role author
author2 Cacho, Juan
Ferreira, Vicente
author2_role author
author
dc.subject.none.fl_str_mv Thiols
Pentafluorobenzylbromide
GC–NCI–MS
topic Thiols
Pentafluorobenzylbromide
GC–NCI–MS
description A fast method for the determination of aroma-powerful polyfunctional thiols at nanogram per liter level has been developed and applied to wine. A small volume of wine (6 mL) was extracted with 1.5 mL of benzene containing four internal standards. Pentafluorobenzyl derivatives of mercaptans were formed in the extract by adding small amounts (100 mg L−1) of pentafluorobenzyl bromide and a strong alkali: 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU). After washing with a water:methanol (5:1) solution 0.5 M in HCl, 20 L of the extract was directly injected into a gas chromatograph. Derivatives were detected by negative ion mass spectrometry. The method makes it possible to simultaneously determine 2-furfurylthiol (2-furanmethanethiol) (FFT), 4-mercapto-4-methyl-2-pentanone (MP), 3-mercaptohexylacetate (MHA) and 3-mercaptohexanol (MH). Inconsistent results were obtained for 2-methyl-3-furanthiol (MF). Detection limits were 0.5 ng L−1 (FFT), 0.1 ng L−1 (MP), 0.6 ng L−1 (MHA) and 7 ng L−1 (MH), well below the corresponding odor detection thresholds. Method repeatability (10% < RSD < 17%) and linearity (0.98 < R2 < 0.999) were satisfactory. The linear range was more than 2 orders of magnitude wide, covering the natural range of occurrence of these compounds in wine, and the slopes of the standard addition plots from different wines were very similar. The different aspects of the method optimization are discussed.
publishDate 2007
dc.date.none.fl_str_mv 2007
dc.type.none.fl_str_mv info:eu-repo/semantics/article
info:eu-repo/semantics/publishedVersion
format article
status_str publishedVersion
dc.identifier.none.fl_str_mv https://doi.org/10.1016/j.chroma.2007.02.003
https://uvadoc.uva.es/handle/10324/73732
url https://doi.org/10.1016/j.chroma.2007.02.003
https://uvadoc.uva.es/handle/10324/73732
dc.language.none.fl_str_mv Inglés
language_invalid_str_mv Inglés
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
http://creativecommons.org/licenses/by-nc-nd/4.0/
eu_rights_str_mv openAccess
rights_invalid_str_mv http://creativecommons.org/licenses/by-nc-nd/4.0/
dc.format.none.fl_str_mv application/pdf
dc.publisher.none.fl_str_mv Elsevier
publisher.none.fl_str_mv Elsevier
dc.source.none.fl_str_mv reponame:UVaDOC. Repositorio Documental de la Universidad de Valladolid
instname:Universidad de Valladolid
instname_str Universidad de Valladolid
reponame_str UVaDOC. Repositorio Documental de la Universidad de Valladolid
collection UVaDOC. Repositorio Documental de la Universidad de Valladolid
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