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Exploring the Volatile Profile of Whiskey Samples using Solid-Phase Microextraction Arrow and Comprehensive Two-Dimensional Gas Chromatography-Mass Spectrometry

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Author(s): Antonio Ferracane1,2, Natalia Manousi2,3, Peter Q. Tranchida1, George A. Zachariadis3, Luigi Mondello1,4,5, Erwin Rosenberg2
1. Department of Chemical, Biological, Pharmaceutical and Environmental Sciences, University of Messina, Messina, Italy, 2. Institute of Chemical Technology and Analytics, Vienna University of Technology, Getreidemarkt 9/164, Vienna 1060, Austria, 3. Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, Thessaloniki 54124, Greece, 4. Chromaleont s.r.l., c/o Department of Chemical, Biological, Pharmaceutical and Environmental Sciences, University of Messina, Messina, Italy, 5. Department of Sciences and Technologies for Human and Environment, University Campus Bio-Medico of Rome, Rome, Italy

Published By: Journal of Chromatography A

Issue: Volume: 1676

Year of Publication: 2022


Abstract: We present a novel sample preparation method for the extraction and preconcentration of volatile organic compounds from whiskey samples prior to their determination by comprehensive two-dimensional gas chromatography (GC × GC) coupled to mass spectrometry (MS). Sample preparation of the volatile compounds, important for the organoleptic characteristics of different whiskeys and their acceptance and liking by the consumers, is based on the use of the solid-phase microextraction (SPME) Arrow. After optimization, the proposed method was compared with conventional SPME regarding the analysis of different types of whiskey (i.e., Irish whiskey, single malt Scotch whiskey and blended Scotch whiskey) and was shown to exhibit an up to a factor of six higher sensitivity and better repeatability by a factor of up to five, depending on the compound class. A total of 167 volatile organic compounds, including terpenes, alcohols, esters, carboxylic acids, ketones, were tentatively-identified using the SPME Arrow technique, while a significantly lower number of compounds (126) were determined by means of conventional SPME. SPME Arrow combined with GC × GC-MS was demonstrated to be a powerful analytical tool for the exploration of the volatile profile of complex samples, allowing to identify differences in important flavour compounds for the three different types of whiskey investigated.

Acknowledgment(s): Support of this work was provided through the Restek Academic Support Program (RASP - Restek, Bellefonte, PA, USA). This analysis also used multiple Restek products including Restek PAL SPME Arrow fibers (cat.# 27487), Restek PAL SPME Manual Injection Kit (cat.# 27490), Rtx-5MS—Low-Bleed GC-MS Columns (cat.# 12623), and Stabilwax-MS GC Columns.


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