Exploring the Extra-Virgin Olive Oil Volatilome by Adding Extra Dimensions to Comprehensive Two-Dimensional Gas Chromatography and Time-of-Flight Mass Spectrometry Featuring Tandem Ionization: Validation of Ripening Markers in Headspace Linearity Conditions.


Journal

Journal of AOAC International
ISSN: 1944-7922
Titre abrégé: J AOAC Int
Pays: England
ID NLM: 9215446

Informations de publication

Date de publication:
21 May 2021
Historique:
received: 25 03 2020
revised: 29 06 2020
accepted: 29 06 2020
entrez: 21 5 2021
pubmed: 22 5 2021
medline: 29 6 2021
Statut: ppublish

Résumé

Comprehensive two-dimensional gas chromatography (GC×GC) combined with time-of-flight (TOF) MS is the most informative analytical approach for chemical characterization of the complex food volatilome. Key analytical features include separation power and resolution enhancement, improved sensitivity, and structured separation patterns from chemically correlated analytes. In this study, we explore the complex extra-virgin olive oil volatilome by combining headspace (HS) solid-phase microextraction (SPME), applied under HS linearity conditions to GC×GC-TOF MS and featuring hard and soft ionization in tandem. Multiple analytical dimensions are combined in a single run and evaluated in terms of chemical dimensionality, method absolute and relative sensitivity, identification reliability provided by spectral signatures acquired at 70 and 12 eV, and dynamic and linear range of response provided by soft ionization. Method effectiveness is validated on a sample set of oils from Picual olives at different ripening stages. Ripening markers [3,4-diethyl-1,5-hexadiene (RS/SR), 3,4-diethyl-1,5-hexadiene (meso), (5Z)-3-ethyl-1,5-octadiene, (5E)-3-ethyl-1,5-octadiene, (E, Z)-3,7-decadiene and (E, E)-3,7-decadiene, (Z)-2-hexenal, (Z)-3-hexenal and (Z)-3-hexenal, (E)-2-pentenal, (Z)-2-pentenal, 1-pentanol, 1-penten-3-ol, 3-pentanone, and 1-penten-3-one] and quality indexes [(Z)-3-hexenal/nonanal, (Z)-3-hexenal/octane, (E)-2-pentenal/nonanal, and (E)-2-pentenal/octane] are confirmed for their validity in HS linearity conditions. For the complex olive oil volatilome, the proposed approach offers concrete advantages for the validation of the informative role of existing analytes while suggesting new potential markers to be studied in larger sample sets. The accurate fingerprinting of volatiles by HS-SPME operating in HS linearity conditions followed by GC×GC-TOF MS featuring tandem ionization gives the opportunity to improve the quality of analytical data and reliability of results.

Sections du résumé

BACKGROUND BACKGROUND
Comprehensive two-dimensional gas chromatography (GC×GC) combined with time-of-flight (TOF) MS is the most informative analytical approach for chemical characterization of the complex food volatilome. Key analytical features include separation power and resolution enhancement, improved sensitivity, and structured separation patterns from chemically correlated analytes.
OBJECTIVE OBJECTIVE
In this study, we explore the complex extra-virgin olive oil volatilome by combining headspace (HS) solid-phase microextraction (SPME), applied under HS linearity conditions to GC×GC-TOF MS and featuring hard and soft ionization in tandem.
METHOD METHODS
Multiple analytical dimensions are combined in a single run and evaluated in terms of chemical dimensionality, method absolute and relative sensitivity, identification reliability provided by spectral signatures acquired at 70 and 12 eV, and dynamic and linear range of response provided by soft ionization.
RESULTS RESULTS
Method effectiveness is validated on a sample set of oils from Picual olives at different ripening stages. Ripening markers [3,4-diethyl-1,5-hexadiene (RS/SR), 3,4-diethyl-1,5-hexadiene (meso), (5Z)-3-ethyl-1,5-octadiene, (5E)-3-ethyl-1,5-octadiene, (E, Z)-3,7-decadiene and (E, E)-3,7-decadiene, (Z)-2-hexenal, (Z)-3-hexenal and (Z)-3-hexenal, (E)-2-pentenal, (Z)-2-pentenal, 1-pentanol, 1-penten-3-ol, 3-pentanone, and 1-penten-3-one] and quality indexes [(Z)-3-hexenal/nonanal, (Z)-3-hexenal/octane, (E)-2-pentenal/nonanal, and (E)-2-pentenal/octane] are confirmed for their validity in HS linearity conditions.
CONCLUSIONS CONCLUSIONS
For the complex olive oil volatilome, the proposed approach offers concrete advantages for the validation of the informative role of existing analytes while suggesting new potential markers to be studied in larger sample sets.
HIGHLIGHTS CONCLUSIONS
The accurate fingerprinting of volatiles by HS-SPME operating in HS linearity conditions followed by GC×GC-TOF MS featuring tandem ionization gives the opportunity to improve the quality of analytical data and reliability of results.

Identifiants

pubmed: 34020455
pii: 5881357
doi: 10.1093/jaoacint/qsaa095
doi:

Substances chimiques

Olive Oil 0
Volatile Organic Compounds 0

Types de publication

Journal Article

Langues

eng

Sous-ensembles de citation

IM

Pagination

274-287

Informations de copyright

© AOAC INTERNATIONAL 2020. All rights reserved. For permissions, please email: journals.permissions@oup.com.

Auteurs

Federico Stilo (F)

Università degli Studi di Torino, Dipartimento di Scienza e Tecnologia del Farmaco, Via Pietro Giuria 9, 10125, Torino, Italy.

Erica Liberto (E)

Università degli Studi di Torino, Dipartimento di Scienza e Tecnologia del Farmaco, Via Pietro Giuria 9, 10125, Torino, Italy.

Stephen E Reichenbach (SE)

GC Image LLC, 201 N 8th Street Unit 420, Lincoln, NE 68508, USA.
University of Nebraska-Lincoln, Computer Science and Engineering Department, 256 Avery Hall, Lincoln, NE 68588, USA.

Qingping Tao (Q)

GC Image LLC, 201 N 8th Street Unit 420, Lincoln, NE 68508, USA.

Carlo Bicchi (C)

Università degli Studi di Torino, Dipartimento di Scienza e Tecnologia del Farmaco, Via Pietro Giuria 9, 10125, Torino, Italy.

Chiara Cordero (C)

Università degli Studi di Torino, Dipartimento di Scienza e Tecnologia del Farmaco, Via Pietro Giuria 9, 10125, Torino, Italy.

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