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

Federico Stilo, Erica Liberto, Stephen E. Reichenbach, Qingping Tao, Carlo Bicchi, Chiara Cordero

Research output: Contribution to journalArticlepeer-review

5 Scopus citations

Abstract

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: 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: 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: 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: 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: 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.

Original languageEnglish (US)
Pages (from-to)274-287
Number of pages14
JournalJournal of AOAC International
Volume104
Issue number2
DOIs
StatePublished - May 21 2021

ASJC Scopus subject areas

  • Analytical Chemistry
  • Food Science
  • Environmental Chemistry
  • Agronomy and Crop Science
  • Pharmacology

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