Next Article in Journal
Heterocycles 38. Biocatalytic Synthesis of New Heterocyclic Mannich Bases and Derivatives
Next Article in Special Issue
Allergenic Proteins in Enology: A Review on Technological Applications and Safety Aspects
Previous Article in Journal
Synthesis and Evaluation of New Podophyllotoxin Derivatives with in Vitro Anticancer Activity
Previous Article in Special Issue
Volatile Compounds from Grape Skin, Juice and Wine from Five Interspecific Hybrid Grape Cultivars Grown in Québec (Canada) for Wine Production
Article Menu

Export Article

Open AccessArticle
Molecules 2015, 20(7), 12280-12299;

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

Department of Food Science, Cornell University, Stocking Hall, 411 Tower Road, Ithaca, NY 14853, USA
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)
Full-Text   |   PDF [2270 KB, uploaded 6 July 2015]   |  


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

Figure 1

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).

Share & Cite This Article

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.

Show more citation formats Show less citations formats

Related Articles

Article Metrics

Article Access Statistics



[Return to top]
Molecules EISSN 1420-3049 Published by MDPI AG, Basel, Switzerland RSS E-Mail Table of Contents Alert
Back to Top