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Molecules 2015, 20(7), 12280-12299; doi:10.3390/molecules200712280

Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation

1
Department of Food Science, Cornell University, Stocking Hall, 411 Tower Road, Ithaca, NY 14853, USA
2
E. & J. Gallo Winery, 600 Yosemite Boulevard, Modesto, CA 95354, USA
*
Author to whom correspondence should be addressed.
Academic Editors: Susan Ebeler and Helene Hopfer
Received: 30 May 2015 / Revised: 29 June 2015 / Accepted: 30 June 2015 / Published: 6 July 2015
(This article belongs to the Collection Wine Chemistry)
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Abstract

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. View Full-Text
Keywords: wine; polyfunctional thiols; extractive alkylation; Vitis labruscana wine; polyfunctional thiols; extractive alkylation; Vitis labruscana
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This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. (CC BY 4.0).

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MDPI and ACS Style

Musumeci, L.E.; Ryona, I.; Pan, B.S.; Loscos, N.; Feng, H.; Cleary, M.T.; Sacks, G.L. Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation. Molecules 2015, 20, 12280-12299.

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