Fingerprinting of the Unsaponifiable Fraction of Vegetable Oils by Using Cryogenically-Modulated Comprehensive Two-Dimen
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Fingerprinting of the Unsaponifiable Fraction of Vegetable Oils by Using Cryogenically-Modulated Comprehensive Two-Dimensional Gas Chromatography-High Resolution Time-of-Flight Mass Spectrometry Ivan Aloisi 1 & Mariosimone Zoccali 2 & Paola Dugo 1,3,4 & Peter Q. Tranchida 1
&
Luigi Mondello 1,3,4,5
Received: 16 April 2020 / Accepted: 10 May 2020 # Springer Science+Business Media, LLC, part of Springer Nature 2020
Abstract The present research is focused on the development of a cryogenically modulated (CM) comprehensive two-dimensional gas chromatography-high resolution time-of-flight mass spectrometry (GC × GC-HR ToFMS) method for the in-depth profiling of the unsaponifiable fraction of vegetable oils. Specifically, twelve vegetable oils (9 extra-virgin olive, soybean, peanut, and hazelnut oils) were subjected to analysis, with particular attention devoted to the higher molecular weight constituents (sterols, vitamin E, triterpenic alcohols). Peak assignment was carried out by using commercial unit-mass MS databases, accurate mass data, literature and on-line freely-available mass spectral information, as well as an in-lab-constructed HR ToFMS lipid database. The main objective of the work was to develop a method to define a well-characterized extra-virgin olive oil fingerprint, to be potentially exploited for vegetable oil differentiation. An additional objective of the investigation was to evaluate the performance of the HR ToFMS system (operated at a mass resolution of 25,000 FWHM) under the challenging analytical conditions of a CM GC × GC-based experiment. The HR ToFMS accurate-mass lipid database was (previously) constructed by acquiring, for the main part, the mass spectra of vegetable oil constituents, well-separated from both the matrix and column bleed background. Keywords Vegetable oils . Unsaponifiable fraction . Extra virgin olive oil . Comprehensive two-dimensional gas chromatography . High resolution time-of-flight mass spectrometry
Introduction Electronic supplementary material The online version of this article (https://doi.org/10.1007/s12161-020-01773-9) contains supplementary material, which is available to authorized users. * Peter Q. Tranchida [email protected] 1
Department of Chemical, Biological, Pharmaceutical and Environmental Sciences, University of Messina, Messina, Italy
2
Department of Mathematical and Computational Sciences, Physical Science and Earth Science, University of Messina, Messina, Italy
3
Chromaleont s.r.l., c/o Department of Chemical, Biological, Pharmaceutical and Environmental Sciences, University of Messina, Messina, Italy
4
Unit of Food Science and Nutrition, Department of Medicine, University Campus Bio-Medico of Rome, Rome, Italy
5
BeSep s.r.l., c/o Department of Chemical, Biological, Pharmaceutical and Environmental Sciences, University of Messina, Messina, Italy
Comprehensive two-dimensional gas chromatography (GC × GC) was first reported in 1991, by Liu and Phillips (Liu and Phillips 1991), whereas the first paper reporting the use of GC × GC in co
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