Multi-class determination of undesirables in aquaculture samples by gas chromatography/tandem mass spectrometry with atmospheric pressure chemical ionization: A novel approach for polycyclic aromatic hydrocarbons

• Published in: Talanta (Oxford) Vol. 172; pp. 109 - 119
• Main Authors: Portolés, T., Garlito, B., Nácher-Mestre, Jaime, Berntssen, M.H.G., Pérez-Sánchez, J.
• Format: Journal Article
• Language: English
• Published: Netherlands Elsevier B.V 01-09-2017
• Subjects: Aquaculture; Atmospheric pressure chemical ionization; Feed; Fish; Gas chromatography; Gas Chromatography-Mass Spectrometry - methods; Polycyclic aromatic hydrocarbons; Polycyclic Aromatic Hydrocarbons - analysis; Polycyclic Aromatic Hydrocarbons - chemistry; Tandem Mass Spectrometry - methods; Triple quadrupole; Water Pollutants, Chemical - analysis; Water Pollutants, Chemical - chemistry; Gas chromatography; Atmospheric pressure chemical ionization; Polycyclic aromatic hydrocarbons; Triple quadrupole; Fish; Aquaculture; Feed
• ISSN: 0039-9140; 1873-3573
• DOI: 10.1016/j.talanta.2017.05.025

In this work, a method for the analysis of 24 PAHs in 19 different matrices, including fish tissues, feeds and feed ingredients, has been developed using gas chromatography coupled to triple quadrupole tandem mass spectrometry with atmospheric pressure chemical ionization source (GC-APCI-MS/MS). The method is based on a modification of the unbuffered QuEChERS method, using freezing as an additional clean-up step and applying a 20-fold dilution factor to the final extract. The procedure was also tested for 15 pesticides and 7 polychlorinated biphenyl (PCB) congeners in order to widen the scope of the method.
The excellent sensitivity and selectivity provided by GC-APCI-MS/MS allowed the dilution of the sample extracts and quantification using calibration with standards in solvent for all the 19 matrices tested. The developed method was evaluated at 2, 5 and 50ngg−1 spiking levels. LOQs were 2ngg−1 for most compounds, and LODs ranged from 0.5 to 2ngg−1.
Analysis of real-world samples revealed the presence of naphthalene, fluorene, phenanthrene, fluoranthene and pyrene at concentration levels ranging from 4.8 to 187ngg−1. No PCBs, DDTs and pesticides were found in fillets from salmon and sea bream.
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•GC-APCI-MS/MS to determine 24 PAHs in 19 different matrices from aquaculture field.•Elimination of matrix effect by a 20-fold dilution factor of the final extract.•Use of solvent calibration due to the excellent sensitivity and selectivity gained.•Use of both M+• and [M+H]+ as an additional value to the selectivity.•LOQs of 2ngg−1 for most compounds, and LODs from 0.5 to 2ngg−1.