Food Analytical Methods

, Volume 11, Issue 8, pp 2056–2065 | Cite as

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

  • Ana I. Freitas
  • Vanda Pereira
  • João M. Leça
  • Ana C. Pereira
  • Francisco Albuquerque
  • José C. Marques


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.


Alcoholic beverages Sotolon Heterocyclic acetals Liquid–liquid extraction Design of experiments 


Funding Information

Vanda Pereira (Post Doc), Ana C. Pereira (Post Doc), and João M. Leça (PhD student) are thankful to the Agência Regional para o Desenvolvimento da Investigação Tecnologia e Inovação (ARDITI) for their grants in the scope of the project M1420-09-5369-FSE-000001. The financial support was given by FEDER (+Conhecimento program, project IMPACT II, MADFDR-01-0190-FEDER-000010).

Compliance with Ethical Standards

Conflict of Interest

Ana I. Freitas declares she has no conflict of interest. Vanda Pereira declares she has no conflict of interest. João M. Leça declares he has no conflict of interest. Ana C. Pereira declares she has no conflict of interest. Francisco Albuquerque is an employee of the Madeira Wine Company, S.A. José C. Marques declares he has no conflict of interest.

Ethical Approval

This article does not contain any studies with human participants or animals performed by any of the authors.

Informed Consent

Not applicable.


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Copyright information

© Springer Science+Business Media, LLC, part of Springer Nature 2018

Authors and Affiliations

  1. 1.Faculty of Exact Sciences and EngineeringUniversity of MadeiraFunchalPortugal
  2. 2.Institute of Nanostructures, Nanomodelling and Nanofabrication (I3N)University of AveiroAveiroPortugal
  3. 3.CIEPQPF, Department of Chemical EngineeringUniversity of CoimbraCoimbraPortugal
  4. 4.Madeira Wine Company, SACaniçalPortugal

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