Validation of a Method for Surveillance of Nanoparticles in Mussels Using Single-Particle Inductively Coupled Plasma-Mass Spectrometry.

BACKGROUND: Determining the concentration of nanoparticles (NPs) in marine organisms is important for evaluating their environmental impact and to assess potential food safety risks to human health. OBJECTIVE: The current work aimed at developing an in-house method based on single-particle inductively coupled plasma-mass spectrometry (SP-ICP-MS) suitable for surveillance of NPs in mussels. METHODS: A new low-cost and simple protease mixture was utilized for sample digestion, and novel open-source data processing was used, establishing detection limits on a statistical basis using false-positive and false-negative probabilities. The method was validated for 30 and 60 nm gold NPs spiked to mussels as a proxy for seafood. RESULTS: Recoveries were 76-77% for particle mass concentration and 94-101% for particle number concentration. Intermediate precision was 8-9% for particle mass concentration and 7-8% for particle number concentration. The detection limit for size was 18 nm, for concentration 1.7 ng/g, and 4.2 × 105 particles/g mussel tissue. CONCLUSION: The performance characteristics of the method were satisfactory compared with numeric Codex criteria. Further, the method was applied to titanium-, chromium- and copper-based particles in mussels. HIGHLIGHTS: The method demonstrates a new practical and cost-effective sample treatment, and streamlined, transparent, and reproducible data treatment for the routine surveillance of NPs in mussels.

Varying temporal trends in the levels of six groups of legacy persistent organic pollutants (POPs) in liver of three gadoid species from the North Sea.

From 2005 to 2019, three gadoid species, Atlantic cod (Gadus morhua), haddock (Melanogrammus aeglefinus) and saithe (Pollachius virens), were sampled approximately every third year in the northeastern part of the North Sea. Liver samples were analyzed to investigate levels and temporal trends of six groups of persistent organic pollutants (POPs): polychlorinated biphenyls (PCBs), dichlorodiphenyltrichloroethane (DDT) and its degradation products, hexachlorocyclohexanes (HCHs), hexachlorobenzene (HCB), trans-nonachlor (TNC), and polybrominated diphenyl ethers (PBDEs). Some of the highest average concentrations were found in cod, the levels otherwise being similar between the three species and mostly below established threshold values. The levels of all the contaminants except HCB and TNC were higher than previously reported for cod and haddock in the Barents Sea. Significantly decreasing levels were found for Σ7PCBs, ΣDDTs, ΣHCHs and Σ15PBDEs in all three species, and for TNC in haddock and saithe, while there was no significant trend for TNC in cod. HCB levels increased significantly in cod and haddock and showed only a minor decrease in saithe. The observed time trends of legacy POPs demonstrate the persistence of some of the studied pollutants despite efforts to eliminate them from the marine environment.

Vertical distribution of inorganic nanoparticles in a Norwegian fjord.

Due to the analytical challenges of detecting and quantifying nanoparticles in seawater, the data on distributions of NPs in the marine environment is limited to qualitative studies or by ensemble measurements subject to various analytical artifacts. Single particle inductively coupled plasma mass spectrometry (SP-ICP-MS) allows determination of individual inorganic NPs at environmentally relevant concentrations, yet only few studies have been conducted on selected elements in surface sea water. Here, a sequential multi-element screening method was developed and implemented to provide a first survey of the horizontal and vertical distributions of inorganic nanoparticles and trace elements in a pristine Norwegian fjord prospect for submarine tailings deposition. Statistical control of false-positive detections while minimizing the size detection limit was ensured using a novel raw signal processing. Scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS) gave confirmative and qualitative information regarding particle morphology and composition. Following SP-ICP-MS screening for particles of 16 elements, particulate Al, Fe, Mn, Pb, Si and Ti were found and determined to mass concentrations in ng/L of 1-399, 1-412, below limit of detection (