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SPME Method Optimized by Box-Behnken Design for Impact Odorants in Reduced Alcohol Wines

1,2,†, 1,2,‡, 1,2,§, 1,3 and 1,2,*
National Wine and Grape Industry Centre, Charles Sturt University, Wagga Wagga, NSW 2650, Australia
School of Agricultural and Wine Sciences, Charles Sturt University, Wagga Wagga, NSW 2650, Australia
School of Psychology, Charles Sturt University, Wagga Wagga, NSW 2650, Australia
Author to whom correspondence should be addressed.
Present Address: University of New South Wales, Sydney, NSW 2052, Australia
Present Address: Horticulture Centre, Tasmanian Institute of Agriculture, University of Tasmania, Prospect, NSW 7250, Australia
Present Address: School of Applied Sciences, RMIT University, Melbourne, VIC 3001, Australia
Foods 2018, 7(8), 127;
Received: 20 July 2018 / Revised: 4 August 2018 / Accepted: 8 August 2018 / Published: 10 August 2018
(This article belongs to the Special Issue Wine Composition and Quality Analysis)
PDF [1621 KB, uploaded 10 August 2018]


The important sampling parameters of a headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) procedure such as the extraction temperature, extraction time, and sample volume were optimized to quantify 23 important impact odorants in reduced alcohol red and white wines. A three-factor design of Box-Behnken experiments was used to determine the optimized sampling conditions for each analyte, and a global optimized condition at every ethanol concentration of interest determined using a desirability function that accounts for a low signal response for compounds. Shiraz and Chardonnay wines were dealcoholized from 13.7 and 12.2% v/v ethanol respectively, to 8 and 5% v/v, using a commercially available membrane-based technology. A sample set of the reduced alcohol wines were also reconstituted to their natural ethanol level to evaluate the effect of the ethanol content reduction on volatile composition. The three-factor Box-Behnken experiment ensured an accurate determination of the headspace concentration of each compound at each ethanol concentration, allowing comparisons between wines at varying ethanol levels to be made. Overall, the results showed that the main effect of extraction temperature was considered the most critical factor when studying the equilibrium of reduced alcohol wine impact odorants. The impact of ethanol reduction upon the concentration of volatile compounds clearly resulted in losses of impact odorants from the wines. The concentration of most analytes decreased with dealcoholization compared to that of the natural samples. Significant differences were also found between the reconstituted volatile composition and 5% v/v reduced alcohol wines, revealing that the dealcoholization effect is the result of a combination between the type of dealcoholization treatment and reduction in wine ethanol content. View Full-Text
Keywords: reduced-alcohol wine; solid-phase microextraction; gas chromatography; chemometrics reduced-alcohol wine; solid-phase microextraction; gas chromatography; chemometrics

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Saha, B.; Longo, R.; Torley, P.; Saliba, A.; Schmidtke, L. SPME Method Optimized by Box-Behnken Design for Impact Odorants in Reduced Alcohol Wines. Foods 2018, 7, 127.

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