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Comprehensive Two-dimensional Gas Chromatography for Analysis of the Volatile Compounds and Fishy Odor Off-flavors from Heated Rapeseed Oil

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Abstract

Lipid oxidation leads to the formation of volatile compounds involved in the aroma of edible oils. Specifically, the use of rapeseed oil for frying causes an emission of off-flavors, characterized by a fishy odor. The aim of the present study was to identify the compounds present in the headspace of degraded rapeseed oil, and in particular, to determine the presence of six compounds commonly considered as responsible for the fishy odor: 1-penten-3-one, 1-octen-3-one, (Z)-4-heptenal, (E,Z)-2,6-nonadienal, (E,Z)-2,4-heptadienal, and (E,Z,Z)-2,4,7-decatrienal. Because of the complexity of the headspace of degraded oils, comprehensive two-dimensional gas chromatography (GC × GC) coupled to mass spectrometry (MS) was the technique of choice, providing a suitable separation power and sensitivity. The extraction of volatile compounds was performed by headspace solid-phase microextraction (HS-SPME). First, three different column sets were evaluated (apolar–polar, polar–apolar, apolar–medium polar) by means of a mixture of 33 standards representative of those involved in the aroma of edible oils. The apolar–polar column set was considered as providing a satisfactory separation with an excellent occupation of the separation space. The developed method was then applied to a real sample of heated rapeseed oil and 110 compounds were identified, which included the six compounds of interest. The contribution of GC × GC in terms sensitivity was evaluated by means of a comparison with analyses in 1D-GC. Finally, the concentrations of the compounds involved in the fishy odor in heated oil were determined.

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Authors and Affiliations

  1. Lesieur, R&D Center, Coudekerque-Branche, France

    Lilia Sghaier, Mickaël Watiez & Sylvie Breton

  2. Department of Analytical, Bioanalytical Sciences and Miniaturization (LSABM), Institute of Chemistry, Biology and Innovation (CBI), ESPCI ParisTech, CNRS UMR 8231, PSL* Research University, 10 rue Vauquelin, 75231, Paris Cedex 05, France

    Lilia Sghaier, Ameline Kopczuk, Patrick Sassiat, Didier Thiebaut & Jérôme Vial

  3. INRA, UMR 1145 GENIAL, Analytical Chemistry Laboratory, 16 rue Claude Bernard, 75005, Paris, France

    Christophe B. Y. Cordella

  4. AgroParisTech, UMR 1145 GENIAL, Analytical Chemistry Laboratory, 16 rue Claude Bernard, 75005, Paris, France

    Lilia Sghaier & Douglas N. Rutledge

Authors
  1. Lilia Sghaier
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  2. Christophe B. Y. Cordella
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  3. Douglas N. Rutledge
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Correspondence to Lilia Sghaier.

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Sghaier, L., Cordella, C.B.Y., Rutledge, D.N. et al. Comprehensive Two-dimensional Gas Chromatography for Analysis of the Volatile Compounds and Fishy Odor Off-flavors from Heated Rapeseed Oil. Chromatographia 78, 805–817 (2015). https://doi.org/10.1007/s10337-015-2897-8

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  • DOI: https://doi.org/10.1007/s10337-015-2897-8

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