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Advisor(s)
Abstract(s)
Sotolon and the heterocyclic acetals of glycerol are known as potential aging and oxidation markers in fortified wines such as
Madeira, Port, and Sherry. Thus, determining the evolution of these compounds under different oxidative aging conditions is
important for fortified wine quality purposes. This study proposes a new methodology based on a miniaturized emulsification
extraction followed by GC–MS/SIM, which was developed and optimized to follow the formation of sotolon and heterocyclic
acetals in fortified wines that were submitted to traditional accelerated aging and micro-oxygenation. The optimization was
achieved by means of a mixed-level factorial design, considering 3 factors: sample volume, extractant volume, and concentrated
extract volume, by performing 19 experiments in duplicate. The extraction was optimized using 8 mL of wine sample, 5 mL of
dichloromethane, concentrating the extract up to 10-fold. The method performance was evaluated for sotolon, using a matrix matched calibration between 10 and 2000 μg/L. The selectivity was confirmed through the analysis of real samples. The
methodology showed good linearity (R2 = 0.999), high sensitivity (LOQ = 6.8 μg/L), recovery about 105%, and good precision
(less than 8 and 9%, evaluated by the variation of intra- and inter-day measurements, respectively). This is the first methodology
that revealed to be an excellent tool to simultaneously follow the formation of sotolon and heterocyclic acetals in Madeira wines,
using an inexpensive, simple, efficient, and effective experimental layout. Indeed, it was shown that traditional accelerated aging
and micro-oxygenation have impact on the formation of such molecules.
Description
Keywords
Alcoholic beverages Sotolon Heterocyclic acetals Liquid–liquid extraction Design of experiments . Escola Superior de Tecnologias e Gestão
Citation
Freitas, A. I., Pereira, V., Leça, J. M., Pereira, A. C., Albuquerque, F., & Marques, J. C. (2018). A simple emulsification-assisted extraction method for the GC–MS/SIM analysis of wine markers of aging and oxidation: application for studying micro-oxygenation in Madeira Wine. Food Analytical Methods, 11(8), 2056-2065. https://doi.org/10.1007/s12161-018-1176-3
Publisher
Springer