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Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation
Analyses of key odorous polyfunctional volatile thiols in wines (3-mercaptohexanol (3-MH), 3-mercaptohexylacetate (3-MHA), and 4-mercapto-4-methyl-2-pentanone (4-MMP)) are challenging due to their high reactivity and ultra-trace concentrations, especially when using conventional gas-chromatography e...
Autores principales: | , , , , , , |
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Formato: | Online Artículo Texto |
Lenguaje: | English |
Publicado: |
MDPI
2015
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Materias: | |
Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC6332517/ https://www.ncbi.nlm.nih.gov/pubmed/26154886 http://dx.doi.org/10.3390/molecules200712280 |
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author | Musumeci, Lauren E. Ryona, Imelda Pan, Bruce S. Loscos, Natalia Feng, Hui Cleary, Michael T. Sacks, Gavin L. |
author_facet | Musumeci, Lauren E. Ryona, Imelda Pan, Bruce S. Loscos, Natalia Feng, Hui Cleary, Michael T. Sacks, Gavin L. |
author_sort | Musumeci, Lauren E. |
collection | PubMed |
description | Analyses of key odorous polyfunctional volatile thiols in wines (3-mercaptohexanol (3-MH), 3-mercaptohexylacetate (3-MHA), and 4-mercapto-4-methyl-2-pentanone (4-MMP)) are challenging due to their high reactivity and ultra-trace concentrations, especially when using conventional gas-chromatography electron impact mass spectrometry (GC-EI-MS). We describe a method in which thiols are converted to pentafluorobenzyl (PFB) derivatives by extractive alkylation and the organic layer is evaporated prior to headspace solid phase microextraction (HS-SPME) and GC-EI-MS analysis. Optimal parameters were determined by response surface area modeling. The addition of NaCl solution to the dried SPME vials prior to extraction resulted in up to less than fivefold improvement in detection limits. Using 40 mL wine samples, limits of detection for 4-MMP, 3-MH, and 3-MHA were 0.9 ng/L, 1 ng/L, and 17 ng/L, respectively. Good recovery (90%–109%) and precision (5%–11% RSD) were achieved in wine matrices. The new method was used to survey polyfunctional thiol concentrations in 61 commercial California and New York State wines produced from V. vinifera (Riesling, Gewürztraminer, Cabernet Sauvignon, Sauvignon blanc and non-varietal rosé wines), V. labruscana (Niagara), and Vitis spp. (Cayuga White). Mean 4-MMP concentrations in New York Niagara (17 ng/L) were not significantly different from concentrations in Sauvignon blanc, but were significantly higher than 4-MMP in other varietal wines. |
format | Online Article Text |
id | pubmed-6332517 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2015 |
publisher | MDPI |
record_format | MEDLINE/PubMed |
spelling | pubmed-63325172019-01-24 Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation Musumeci, Lauren E. Ryona, Imelda Pan, Bruce S. Loscos, Natalia Feng, Hui Cleary, Michael T. Sacks, Gavin L. Molecules Article Analyses of key odorous polyfunctional volatile thiols in wines (3-mercaptohexanol (3-MH), 3-mercaptohexylacetate (3-MHA), and 4-mercapto-4-methyl-2-pentanone (4-MMP)) are challenging due to their high reactivity and ultra-trace concentrations, especially when using conventional gas-chromatography electron impact mass spectrometry (GC-EI-MS). We describe a method in which thiols are converted to pentafluorobenzyl (PFB) derivatives by extractive alkylation and the organic layer is evaporated prior to headspace solid phase microextraction (HS-SPME) and GC-EI-MS analysis. Optimal parameters were determined by response surface area modeling. The addition of NaCl solution to the dried SPME vials prior to extraction resulted in up to less than fivefold improvement in detection limits. Using 40 mL wine samples, limits of detection for 4-MMP, 3-MH, and 3-MHA were 0.9 ng/L, 1 ng/L, and 17 ng/L, respectively. Good recovery (90%–109%) and precision (5%–11% RSD) were achieved in wine matrices. The new method was used to survey polyfunctional thiol concentrations in 61 commercial California and New York State wines produced from V. vinifera (Riesling, Gewürztraminer, Cabernet Sauvignon, Sauvignon blanc and non-varietal rosé wines), V. labruscana (Niagara), and Vitis spp. (Cayuga White). Mean 4-MMP concentrations in New York Niagara (17 ng/L) were not significantly different from concentrations in Sauvignon blanc, but were significantly higher than 4-MMP in other varietal wines. MDPI 2015-07-06 /pmc/articles/PMC6332517/ /pubmed/26154886 http://dx.doi.org/10.3390/molecules200712280 Text en © 2015 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution license (http://creativecommons.org/licenses/by/4.0/). |
spellingShingle | Article Musumeci, Lauren E. Ryona, Imelda Pan, Bruce S. Loscos, Natalia Feng, Hui Cleary, Michael T. Sacks, Gavin L. Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation |
title | Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation |
title_full | Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation |
title_fullStr | Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation |
title_full_unstemmed | Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation |
title_short | Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation |
title_sort | quantification of polyfunctional thiols in wine by hs-spme-gc-ms following extractive alkylation |
topic | Article |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC6332517/ https://www.ncbi.nlm.nih.gov/pubmed/26154886 http://dx.doi.org/10.3390/molecules200712280 |
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