title: Direct-immersion solid-phase microextraction coupled to fast gas chromatography mass spectrometry as a purification step for polycyclic aromatic hydrocarbons determination in olive oil.
abstract: The aim of the present work was to optimize a preparation step for polycyclic aromatic hydrocarbons in a fatty extract. Solid-phase microextraction is an easy preparation technique, which allows to minimize solvent consumption and reduce sample manipulation. A Carbopack Z/polydimethylsiloxane fiber, particularly suitable for extraction of planar compounds, was employed to extract polycyclic aromatic hydrocarbons from a hexane solution obtained after a previous extraction with acetonitrile from oil, followed by a liquid-liquid partition between acetonitrile and hexane. The proposed method was a rapid and sensitive solution to reduce the interference of triglycerides saving the column life and avoiding frequent cleaning of the mass spectrometer ion source. Despite the non-quantitative extraction of polycyclic aromatic hydrocarbons from oil using acetonitrile, the signal-to-noise ratio was significantly improved obtaining a limit of detection largely below the performance criteria required by the European Union legislation.
authors.affiliation: Dipartimento di Scienze degli Alimenti, University of Udine, via Sondrio 2/A, 33100 Udine, Italy. giopurcaro@gmail.com
authors.forename: Giorgia
authors.initials: G
authors.lastname: Purcaro
authors.forename: Massimo
authors.initials: M
authors.lastname: Picardo
authors.forename: Laura
authors.initials: L
authors.lastname: Barp
authors.forename: Sabrina
authors.initials: S
authors.lastname: Moret
authors.forename: Lanfranco S
authors.initials: LS
authors.lastname: Conte
mesh_terms: D000097:Acetonitriles / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D057230:Limit of Detection; D000069463:Olive Oil; D010938:Plant Oils / Q000737:chemistry*; D011084:Polycyclic Aromatic Hydrocarbons / Q000032:analysis* / Q000302:isolation & purification; D015203:Reproducibility of Results; D052617:Solid Phase Microextraction / Q000379:methods*; D015040:Zirconium / Q000737:chemistry
chemical_list: D000097:Acetonitriles; D000069463:Olive Oil; D010938:Plant Oils; D011084:Polycyclic Aromatic Hydrocarbons; D015040:Zirconium; C028541:zirconium oxide; C032159:acetonitrile
keywords: Direct immersion (DI); Edible oil; Gas chromatography–mass spectrometry (GC–MS); Polycyclic aromatic hydrocarbons (PAHs); Solid-phase microextraction (SPME); Zirconia-based sorbent (Z-Sep+)