title: A reliable analytical approach based on gas chromatography coupled to triple quadrupole and time-of-flight mass analyzers for the determination and confirmation of polycyclic aromatic hydrocarbons in complex matrices from aquaculture activities.
abstract: The potential of gas chromatography coupled to tandem mass spectrometry (GC/MS/MS) with a triple quadrupole analyzer (QqQ) has been investigated for the quantification and reliable identification of sixteen polycyclic aromatic hydrocarbons (PAHs) from the EPA priority list in animal and vegetable samples from aquaculture activities, whose fat content ranged from 5 to 100%. Matrices analyzed included fish fillet, fish feed, fish oil and linseed oil. Combining optimized saponification and solid-phase extraction led to high efficiency in the elimination of interfering compounds, mainly fat, from the extracts. The developed procedure minimized the presence of these interfering compounds in the extracts and provided satisfactory recoveries of PAHs. The excellent sensitivity and selectivity of GC/(QqQ)MS/MS in selected reaction monitoring (SRM) allowed to reach limits of detection at pg/g levels. Two SRM transitions were acquired for each analyte to ensure reliable identification of compounds detected in samples. Confirmation of positive findings was performed by GC coupled to high-resolution time-of-flight mass spectrometry (GC/TOFMS). The accurate mass information provided by GC/TOFMS in full acquisition mode together with its high mass resolution makes it a powerful analytical tool for the unequivocal confirmation of PAHs in the matrices tested. The method developed was applied to the analysis of real-world samples of each matrix studied with the result of detecting and confirming the majority of analytes at the microg/kg level by both QqQ and TOF mass spectrometers.
authors.affiliation: Research Institute for Pesticides and Water (IUPA), Avda Sos Baynat, s/n. University Jaume I, 12071 Castellón, Spain.
authors.forename: Jaime
authors.initials: J
authors.lastname: Nácher-Mestre
authors.forename: Roque
authors.initials: R
authors.lastname: Serrano
authors.forename: Tania
authors.initials: T
authors.lastname: Portolés-Nicolau
authors.forename: Félix
authors.initials: F
authors.lastname: Hernández
authors.forename: Laura
authors.initials: L
authors.lastname: Benedito-Palos
authors.forename: Jaume
authors.initials: J
authors.lastname: Pérez-Sánchez
mesh_terms: D000818:Animals; D005396:Fish Products / Q000032:analysis; D005399:Fishes; D008401:Gas Chromatography-Mass Spectrometry / Q000295:instrumentation / Q000379:methods*; D008460:Meat / Q000032:analysis; D011084:Polycyclic Aromatic Hydrocarbons / Q000032:analysis*; D053719:Tandem Mass Spectrometry / Q000295:instrumentation / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D011084:Polycyclic Aromatic Hydrocarbons; D014874:Water Pollutants, Chemical