title: Multiscreening determination of organic pollutants in molluscs using matrix solid phase dispersion.
abstract: This work describes the optimisation, validation and application of matrix solid-phase dispersion (MSPD) coupled to gas chromatography mass spectrometry, both single quadrupole (GC-MS) and tandem (GC-MS/MS), for the quantification in molluscs of up to 40 different analytes belonging to several families of priority and emerging organic contaminants, including polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), polybrominated diphenyl ethers (PBDEs), organochlorine pesticides (OCPs), organophosphorus pesticides (OPPs) and musk fragrances. The MSPD procedure was fully optimised with a special focus on the clean-up strategy. The best recoveries were obtained using glass syringes, 0.30 g of freeze-dried sample, 0.30 g of Florisil as solid support, 4.00 g of activated silica and 25 mL of dichloromethane as elution solvent. Using GC-MS/MS the method afforded good linearities (r(2), between 0.980 and 0.9996), adequate repeatability and reproducibility (RSD<17% and 33%, respectively) and low instrumental limits of detection (between 0.010 and 2.74 ng mL(-1)). The accuracy of the method was evaluated using different approaches, i.e. assessment of spiked fish hatchery samples, laboratory reference material and standard reference material (SRM 2977). Satisfactory apparent recoveries were obtained for all the target analytes after correction with the corresponding labelled surrogate, except for PAHs in the case of SRM 2977, which required the use of the standard addition method. Finally, MSPD was applied to mollusc species collected in Colombia and Nicaragua, where PAHs, PCBs, musks and pesticides were detected at low ng g(-1) levels.
authors: Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), P.O. Box 644, 48080 Bilbao, Spain. Electronic address: h.ziarrusta@gmail.com.
authors: H
authors: H
authors: Ziarrusta
authors: Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), P.O. Box 644, 48080 Bilbao, Spain.
authors: M
authors: M
authors: Olivares
authors: Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), P.O. Box 644, 48080 Bilbao, Spain.
authors: A
authors: A
authors: Delgado
authors: Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), P.O. Box 644, 48080 Bilbao, Spain.
authors: O
authors: O
authors: Posada-Ureta
authors: Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), P.O. Box 644, 48080 Bilbao, Spain.
authors: O
authors: O
authors: Zuloaga
authors: Department of Analytical Chemistry, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), P.O. Box 644, 48080 Bilbao, Spain.
authors: N
authors: N
authors: Etxebarria
mesh_terms: D000818:Animals; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D055768:Halogenated Diphenyl Ethers / Q000032:analysis; D006843:Hydrocarbons, Chlorinated / Q000032:analysis; D008974:Mollusca / Q000737:chemistry*; D010476:Perfume / Q000032:analysis; D010575:Pesticides / Q000032:analysis; D011078:Polychlorinated Biphenyls / Q000032:analysis; D011084:Polycyclic Aromatic Hydrocarbons / Q000032:analysis; D015203:Reproducibility of Results; D053719:Tandem Mass Spectrometry / Q000379:methods; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D055768:Halogenated Diphenyl Ethers; D006843:Hydrocarbons, Chlorinated; D010476:Perfume; D010575:Pesticides; D011084:Polycyclic Aromatic Hydrocarbons; D014874:Water Pollutants, Chemical; D011078:Polychlorinated Biphenyls
keywords: Gas chromatography–tandem mass spectrometry; Matrix solid phase dispersion; Molluscs; Multiresidue extraction; Organic pollutants