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A Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method has been adapted and validated for the simultaneous analysis of 16 PAHs, 12 PCBs and 9 OCPs in sediment. The sample preparation was adapted by modifying the nature of the extraction solvent, the extraction technique and the amount of sediment. The analytical performances were evaluated in terms of accuracy, linearity and quantification limits. The method was validated by the analysis of a reference marine sediment material (SRM 1941b). The obtained concentrations are in good agreement with the certified values with recoveries ranging 60 %–103 % for most of PAHs. Acceptable recoveries are obtained for PCBs, ranging 76 %–131 %, and for OCPs ranging 81 %–137 %. The method was applied to the analysis of sediments from the hydro-system Bizerte Lagoon/Ichkeul Lake (Tunisia). The Bizerte lagoon is mainly contaminated by PAHs whereas the Ichkeul lake is mainly by OCPs.

As methylmercury (MeHg) can be bioaccumulated and biomagnified in the trophic web, its toxicity for marine mammals is of major concern. Mercury speciation in marine biota has been widely studied, mainly focused on the discrimination and quantification of inorganic Hg and MeHg. Less attention has been paid to the interactions of Hg with biomolecules and the characterization of its specific binding, which play a key role in metabolic pathways controlling its uptake, transformation, and toxicity. In the studied white-sided dolphin ( Lagenorhynchus acutus ) liver homogenate (QC04LH4) sample, approximately 60 % of the total MeHg was found in the water soluble fraction, specifically associated with high molecular weight biomolecules. The identity of the involved proteins was investigated (after tryptic digestion of the fraction) by μRPLC with parallel detection by ICP-MS and ESI-MS/MS. Molecular mass spectrometry experiments were carried out at high resolution (100000) to ensure accurate protein identification and determination of the MeHg binding sites. Cysteine residue on the dolphin hemoglobin β chain was found to be the main MeHg binding site, suggesting that hemoglobin is a major MeHg binding protein in this marine mammal and could be a potential carrier of this MeHg from blood to liver prior to its degradation in this organ. In parallel, a significant proportion of selenium was found to be present as selenoneine and a potential role for this compound in Hg detoxification is discussed.

Dramatic increases in global mercury pollution require a deeper understanding of specific toxicity mechanisms for mercury compounds in organisms. Despite numerous studies addressing mercury toxicity, the detailed mechanisms underlying its transport and accumulation in fish remain unclear. The aim of this study was to unravel differential uptake pathways for mercury compounds, metabolisation, and sequestration mechanisms in glass eels using techniques able to localize at the tissue and organ levels. A multi isotope image mapping procedure was developed to simultaneously study the uptake and distribution of both mercury compounds MeHg and Hg(II) within the organs of the whole organism. The use of isotopically labelled Hg species (methylmercury Me201Hg and inorganic mercury 199Hg(II)) and image based on isotope ratio instead of elemental signals allowed to visualize spatially and with time the differential Hg species uptake, transport, and sequestration routes. The results showed a preferential uptake of the MeHg counterpart and a dynamic transport of MeHg within different organs. The gills were the main target organs for MeHg uptake, whereas the skeletal muscle was the final MeHg storage tissue. Hg(II) was found to mainly transit by the gills and the olfactory bulbs with a very low transfer and storage in the other organs and a rapid depuration. No significant internal demethylation and methylation was observed during this experimentation.

The freshwater lakes of southwestern France are subject to the development of invasive macrophytes which are associated with mercury (Hg) contamination of the food web. The aim of this study was to determine the bioavailability of methylmercury (MeHg) produced by plant roots in aquatic ecosystems. A microcosm experiment was performed using isotopically enriched inorganic Hg at environmental concentrations (1 µg 199IHg·L−1). For all conditions, total Hg in fish as well as Hg species associated with different compartments (water, sediments, plant roots, fish) were analyzed by gas chromatography-inductively coupled plasma-mass spectrometry (GC-ICP-MS). In addition, sediment, plants, and fish gut microbiota were studied by MiSEQ sequencing. Some strains were isolated and tested for their ability to methylate Hg. The results revealed 199MeHg production in plant roots and the presence of this form in fish (tissues and gut), highlighting a MeHg trophic transfer. Moreover, methylator bacteria were identified from the gut contents of the fish when they were in the presence of plants. Some of them were related to bacteria found in the plant roots. On the basis of these results, the transfer of MeHg and bacteria from plants to fish is highlighted; in addition, Hg methylation is strongly suspected in the fish gut, potentially increasing the Hg bioaccumulation.

The analysis of micro- and nanoplastics (MNPs) in the environment is a critical objective due to their ubiquitous presence in natural habitats, as well as their occurrence in various food, beverage, and organism matrices. MNPs pose significant concerns due to their direct toxicological effects and their potential to serve as carriers for hazardous organic/inorganic contaminants and pathogens, thereby posing risks to both human health and ecosystem integrity. Understanding the fate of MNPs within wastewater treatment plants (WWTPs) holds paramount importance, as these facilities can be significant sources of MNP emissions. Additionally, during wastewater purification processes, MNPs can accumulate contaminants and pathogens, potentially transferring them into receiving water bodies. Hence, establishing a robust analytical framework encompassing sampling, extraction, and instrumental analysis is indispensable for monitoring MNP pollution and assessing associated risks. This comprehensive review critically evaluates the strengths and limitations of commonly employed methods for studying MNPs in wastewater, sludge, and analogous environmental samples. Furthermore, this paper proposes potential solutions to address identified methodological shortcomings. Lastly, a dedicated section investigates the association of plastic particles with chemicals and pathogens, alongside the analytical techniques employed to study such interactions. The insights generated from this work can be valuable reference material for both the scientific research community and environmental monitoring and management authorities. Graphical Abstract

Mercury (Hg) is a global pollutant of environmental and health concern; its methylated form, methylmercury (MeHg), is a potent neurotoxin. Sulfur-containing molecules play a role in MeHg production by microorganisms. While sulfides are considered to limit Hg methylation, sulfate and cysteine were shown to favor this process. However, these two forms can be endogenously converted by microorganisms into sulfide. Here, we explore the effect of sulfide (produced by the cell or supplied exogenously) on Hg methylation. For this purpose, Pseudodesulfovibrio hydrargyri BerOc1 was cultivated in non-sulfidogenic conditions with addition of cysteine and sulfide as well as in sulfidogenic conditions. We report that Hg methylation depends on sulfide concentration in the culture and the sulfides produced by cysteine degradation or sulfate reduction could affect the Hg methylation pattern. Hg methylation was independent of hgcA expression. Interestingly, MeHg production was maximal at 0.1–0.5 mM of sulfides. Besides, a strong positive correlation between MeHg in the extracellular medium and the increase of sulfide concentrations was observed, suggesting a facilitated MeHg export with sulfide and/or higher desorption from the cell. We suggest that sulfides (exogenous or endogenous) play a key role in controlling mercury methylation and should be considered when investigating the impact of Hg in natural environments.

The proteins encoded by the hgcA and hgcB genes are currently the only ones known to be involved in the mercury methylation by anaerobic microorganisms. However, no studies have been published to determine the relationships between their expression level and the net/gross methylmercury production. This study aimed to decipher the effect of growth conditions on methylmercury production and the relationships between hgcA and hgcB expression levels and net methylation. Desulfovibrio dechloroacetivorans strain BerOc1 was grown under sulfidogenic conditions with different carbon sources and electron donors as well as under fumarate respiration. A good correlation was found between the biomass production and the methylmercury production when the strain was grown under sulfate-reducing conditions. Methylmercury production was much higher under fumarate respiration when no sulfide was produced. During exponential growth, hgcA and hgcB gene expression levels were only slightly higher in the presence of inorganic mercury, and it was difficult to conclude whether there was a significant induction of hgcA and hgcB genes by inorganic mercury. Besides, no relationships between hgcA and hgcB expression levels and net mercury methylation could be observed when the strain was grown either under sulfate reduction or fumarate respiration, indicating that environmental factors had more influence than expression levels.

To achieve a “Good Environmental Status by 2015,” as demanded by the water framework directive, monitoring programs are needed to furnish data on target compounds. In this study, a first evaluation of influents and main emissions of 3 local wastewater treatment plants (WWTP) in the Adour estuary (southwest of France) was performed for 23 pollutants (10 musk fragrances, 5 alkylphenols, and 8 organometallics), as well as receiving estuarine water from the same area. High frequency of occurrence of these compounds was found in influents samples (musks: 22–100%; alkylphenols 11–100%; organometallics 0–100%) and effluents (musks: 0–100%; alkylphenols 0–100%; organometallics 0–100%). The removal efficiencies were calculated and varied from negative values up to 98% with the lowest values for synthetic musk compounds. Temporal variability of the target compounds also was studied, and a few tendencies were observed. Estimation of the daily output of each WWTP into the estuary also showed that galaxolide, nonylphenol, monobuthyltin, and inorganic mercury were the compounds discharged into the environment at the highest concentrations. Finally, the occurrence of these compounds in estuarine waters was evaluated; most of them were present at concentrations below the limits of quantification (musks: 0.53–41.5 ng/L; alkylphenols 3.4–410 ng/L; organometallics 0.02–0.70 ng/L) suggesting a low impact in the resulting receiving waters.

A new analytical method for the simultaneous determination of eight synthetic musks compounds (SMs) including five polycyclic musks (PCMs) and three nitro musks (NMs) was validated for sediment samples based on a simple QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation procedure followed by gas chromatography–mass spectrometry (GC–MS). Good analytical performances were obtained for all the target compounds. For the validation of the method, internal calibration (IC) and internal calibration with QuEChERS (ICQ) were compared. Good linearity was obtained for both calibration methods with determination coefficients (R 2 ) ranging between 0.990 for Musk Xylene (MX) and 0.999 for Tonalide (AHTN) with IC and between 0.991 for Musk Ketone (MK) and 0.999 for Traseolide (ATII) with ICQ. The repeatability ranges were 0.1 %–1.9 % with the IC and 0.1 %–2.6 % with the ICQ. The apparent recoveries obtained for SMs in the standard reference sediment (SRM1944) varied in the range of 70 %–98 % and 75 %–103 % in the sediment from the Bizerte Lagoon (Tunisia). The absolute recoveries ranged between 61 % and 92 % for the SRM1944 and between 61 % and 89 % in the sediment from the Bizerte Lagoon. The limits of detection (LOD) calculated for the two main compounds, Galaxolide (HHCB) and Tonalide (AHTN) were 0.3 and 0.1 ng g −1 respectively. The LODs obtained for ADBI (Celestolide), AHMI (Phantolide), ATII (Traseolide), MM (Muks mosken), MK (Musk Ketone) and MX (Musk Xylene) were 0.08, 0.12, 0.03, 0.34, 0.11, 0.08, 0.10 and 0.15 ng g −1 respectively. The levels of ∑SMs in surface sediments from the Bizerte Lagoon ranged from 1.4 to 4.5 ng g −1 , which are 1000 times lower that the predicted no effect concentration (PNEC) for marine organisms.

This study aimed to identify the most commonly used agricultural pesticides around Ichkeul Lake–Bizerta Lagoon watershed. First survey of pesticide use on agricultural watershed was performed with farmers, Regional Commissioner for Agricultural Development, and pesticide dealers. Then, sediment contamination by pesticides and response of benthic communities (bacteria and free-living marine nematode) were investigated. The analysis of 22 active organochlorine pesticides in sediments was performed according to quick, easy, cheap, effective, rugged, and safe (QuEChERS) method, biodiversity of indigenous bacterial community sediment was determined by terminal restriction fragment length polymorphism (T-RFLP), and free-living marine nematodes were counted. The results of the field survey showed that iodosulfuron, mesosulfuron, 2,4-dichlorophenoxyacetic acid (2,4 D), glyphosate, and fenoxaprops were the most used herbicides, tebuconazole and epoxiconazole the most used fungicides, and deltamethrin the most used insecticide. Sixteen organochlorine pesticide compounds among the 22 examined were detected in sediments up to 2 ppm in Ichkeul Lake, endrin, dieldrin, and hexachlorocyclohexane being the most detected molecules. The most pesticide-contaminated site in the lake presented the higher density of nematode, but when considering all sites, no clear correlation with organochlorine pesticide (OCP) content could be established. The bacterial community structure in the most contaminated site in the lake was characterized by the terminal restriction fragments (T-RFs) 97, 146, 258, 285, and 335 while the most contaminated site in the lagoon was characterized by the T-RFs 54, 263, 315, 403, and 428. Interestingly, T-RFs 38 and 143 were found in the most contaminated sites of both lake and lagoon ecosystems, indicating that they were resistant to OCPs and able to cope with environmental fluctuation of salinity. In contrast, the T-RFs 63, 100, 118, and 381 in the lake and the T-RFs 40, 60, 80, 158, 300, 321, and 357 in the lagoon were sensitive to OCPs. This study highlighted that the intensive use of pesticides in agriculture, through transfer to aquatic ecosystem, may disturb the benthic ecosystem functioning of the protected area. The free-living marine nematodes and bacterial communities represent useful proxy to follow the ecosystem health and its capacity of resilience.