A Multifaceted investigation of the effect of reduced pressure condition on the headspace-solid phase microextraction of extra-virgin olive oil

Mascrez, Steven; Psillakis, Elefteria; Purcaro, Giorgia

doi:10.1016/j.aca.2019.12.053

Article (Scientific journals)

A Multifaceted investigation of the effect of reduced pressure condition on the headspace-solid phase microextraction of extra-virgin olive oil

Mascrez, Steven; Psillakis, Elefteria; Purcaro, Giorgia

2020 • In Analytica Chimica Acta, 1103, p. 106-114

Peer Reviewed verified by ORBi

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https://hdl.handle.net/2268/257366

DOI
10.1016/j.aca.2019.12.053

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32081174

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Keywords :

Headspace solid-phase microextraction; Vacuum-assisted headspace solid-phase; microextraction; Extra-virgin olive oil; Central composite design

Abstract :

[en] Headspace solid-phase microextraction (HS-SPME) is an easy, effective, and selective technique for the extraction of volatiles and semi-volatiles compounds. For the latter, longer equilibration times are needed, which are typically shortened by applying agitation or heating the sample. A less explored way to improve the extraction kinetics of analytes with a low-affinity for the headspace is to sample under vacuum conditions. The methodology that evolved from this approach was termed “vacuum-assisted HSSPME” (VaceHSeSPME) and was mainly used for water- and solid-based samples. The aim of this work was to investigate the effect of vacuum when dealing with non-aqueous liquid samples. For this purpose, the volatile profile of extra virgin olive oil was analyzed using a divinylbenzene/ carboxen/polydimethylsiloxane fiber followed by gas chromatography-mass spectrometry. The effects of extraction temperature and sampling time were investigated using traditional one-variable at a time approach and a two-variable central component design for both VaceHSeSPME and regular HSSPME. The results showed an important enhancement in the extraction of semi-volatile compounds when using VaceHSeSPME, and improved the information gained for the olive oil aroma fingerprint. A theoretical formulation of the underlying process was proposed, providing new insights into the SPME extraction theory. Lowering the sampling pressure effectively reduced gas-sided limitations and accelerated extraction kinetics. However, for viscous samples such as olive oils, the liquid-phase resistance played an important role and delayed extraction. Overall, applying heating (i.e. reducing the viscosity of the oily sample and increasing headspace concentrations) next to reducing the total pressure in the headspace is the best analytical HS-SPME strategy for obtaining fast a rich volatile profile from the oily samples.

Disciplines :

Chemistry
Food science

Author, co-author :

Mascrez, Steven ; Université de Liège - ULiège > Département GxABT > Chimie des agro-biosystèmes

Psillakis, Elefteria; Technical University of Crete > School of environmental engineering

Purcaro, Giorgia ; Université de Liège - ULiège > Département GxABT > Chimie des agro-biosystèmes

Language :

English

Title :

A Multifaceted investigation of the effect of reduced pressure condition on the headspace-solid phase microextraction of extra-virgin olive oil

Publication date :

2020

Journal title :

Analytica Chimica Acta

ISSN :

0003-2670

eISSN :

1873-4324

Publisher :

Elsevier, Netherlands

Volume :

1103

Pages :

106-114

Peer reviewed :

Peer Reviewed verified by ORBi

Additional URL :

http://portasap.eu/action.html

Name of the research project :

PortASAP - European network for the promotion of portable, affordable and simple analytical platforms

Funders :

COST - European Cooperation in Science and Technology

Available on ORBi :

since 25 February 2021

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