Multiscreening determination of organic pollutants in molluscs using matrix solid phase dispersion

• MSPD for the extraction of PAHs, PCBs, PBDEs, OCPs, OPPs and musks in molluscs.
• All the factors affecting the whole procedure were assessed and optimised.
• Different strategies were evaluated to minimise the matrix effects.
• GC–MS and GC–MS/MS were compared for the simultaneous analysis of 40 compounds.
• The developed method was applied to different mollusc species.

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 (r2, 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.