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- Determination of phthalic acid esters and di(2-ethylhexyl) adipate in fish and squid using the ammonium formate version of the QuEChERS method combined with gas chromatography mass spectrometryPublication . Sambolino, Annalisa; Ortega-Zamora, Cecilia; González-Sálamo, Javier; Dinis, Ana; Cordeiro, Nereida; Canning-Clode, João; Hernández-Borges, JavierIn the present study, the ammonium formate version of the QuEChERS method, considered highly advantageous in relation to instrument maintenance and other issues, was applied for the first time to extract a group of twelve phthalic acid esters (PAEs, i.e. dipropyl phthalate, DPP; diisobutyl phthalate, DIBP; dibutyl phthalate, DBP; diisopentyl phthalate, DIPP; di-n-pentyl phthalate, DNPP; dihexyl phthalate, DHP; butyl benzyl phthalate, BBP; dicyclohexyl phthalate, DCHP; di(2-ethylhexyl) phthalate, DEHP; di-n-octyl phthalate, DNOP; diisononyl phthalate, DINP; and diisodecyl phthalate, DIDP) and one adipate (di(2-ethylhexyl) adipate, DEHA) from two species of fish (Scomber colias and Katsuwonus pelamis) and one of squid (Loligo gahi). The method was validated in terms of linearity, trueness and matrix effects. Determination coefficients (R2 ) for matrix-matched calibration curves were higher than 0.99 in all cases, being the lowest calibration levels in the range 0.5–10 ng/g. Mean recovery values were between 70 and 117% with relative standard deviation values ≤20%. Matrix effects were soft (between − 20 and +20%) for most analytes and matrices, except in squid samples, which was mostly medium with a moderate ion suppression. The analysis of 10 samples of each type showed the presence of DIBP, DBP and DEHP at concentrations up to 44.2 ± 2.1 ng/g of wet weight in some of the samples and species, still not representing concerning values when considering the daily intake of such species of seafood in the human diet (tolerable daily intake -TDI- values were not exceeded). Results demonstrated that the ammonium formate version of the QuEChERS method can be applied with success for the extraction and determination of the selected PAEs and DEHA in fish and squid samples.
- Optimization and validation of a micro–QuEChERS method for phthalates detection in small samples of cetacean blubberPublication . Sambolino, Annalisa; Rodriguez, Marta; De la Fuente, Jesus; Arbelo, Manuel; Fernández, Antonio; Kaufmann, Manfred; Cordeiro, Nereida; Dinis, AnaIn this study, an innovative method was developed to detect and quantify phthalates in fresh cetacean blubber. An adaptation of the ammonium formate QuEChERS method was used and adapted as a micro-extraction for small quantities of samples. Significantly, this technique utilized minimal quantities of reagents and salts, with the additional implementation of rigorous Quality Assurance/Quality Control protocols to further reduce background contamination. To ensure the reliability of this method, comprehensive validation procedures were conducted, with a specific focus on two widely studied cetacean species: the common bottlenose dolphin (Tursiops truncatus) and the short-finned pilot whale (Globicephala macrorhynchus). Determination coefficients (R2) for matrix-matched calibration were >0.93 with limits of quantifications (LOQ) of the method in the range of 5–10 ng/g. Mean recovery values were between 40 and 100 %. This novel methodology holds particular relevance for environmental research studies, offering the capability to detect emerging contaminants with minimal sample requirements. This aspect is particularly valuable in investigations that involve free-ranging animals and rely on biopsy sampling. It allows for the assessment of contaminant levels in healthy individuals within wild populations, enhancing our understanding of ecological impacts and potential conservation measures. • A micro-extraction adaptation of the ammonium formate QuEChERS method was developed and applied to a small quantity of fresh cetacean blubber to detect phthalates. • Small quantities of reagents and salts were used, and additional Quality Assurance/ Quality Control procedures were taken to further minimize background contamination. • Method validation was carried out for two cosmopolitan and extensively studied cetacean species: the common bottlenose dolphin (Tursiops truncatus) and the short-finned pilot whale (Globicephala macrorhynchus).
- Microplastic ingestion and plastic additive detection in pelagic squid and fish: implications for bioindicators and plastic tracers in open oceanic food websPublication . Sambolino, Annalisa; Iniguez, Eva; Herrera, Inma; Kaufmann, Manfred ; Dinis, Ana; Cordeiro, Nereida ; Sambolino, Annalisa; Iñiguez Santamaría, Eva; Kaufmann, Manfred; cordeiro, nereidaThe ubiquitous presence of microplastics (MPs) in the ocean represents a potential threat to marine organisms, with poorly understood long-term adverse effects, including exposure to plastic additives. The present study investigated the ingestion of MPs in two epipelagic fish species (Trachurus picturatus and Scomber colias) and three pelagic squid spe cies (Loligo vulgaris, Ommastrephes caroli and Sthenoteuthis pteropus) from an open oceanic region of the Northeast Atlan tic. Seven phthalate esters (PAEs) were also analysed in the organisms' tissue, and the potential correlation between PAEs concentrations and ingested MPs was investigated. Seventy-two fish and 20 squid specimens were collected and analysed. MPs were found in the digestive tract of all species and in the squid species' gills and ink sacs. The highest occurrence of MPs was in the stomach of S. colias (85 %) and the lowest in the stomach and ink sac of O. caroli and L. vulgaris (12 %). Most of the particles identified (>90 %) were fibres. Among all the ecological and biological factors considered (dietary preferences, season, body size, total weight, liver weight, hepatosomatic index and gastrosomatic index), only gastrosomatic index (GSI) and season were significant predictors of MPs ingestion in fish species, with a greater likelihood of ingestion in the cold season and in specimens with higher GSI values (i.e. higher feeding inten sity). Four PAEs (DEP, DIBP, BBP, DEHP) were detected in all the species analysed, with average ∑PAEs concentrations ranging between 10.31 and 30.86 ng/g (wet weight). DIBP was positively correlated with ingested MPs, suggesting this compound might represent a “plastic tracer”. This study looks into the problem of MPs ingestion for pelagic species in an open oceanic region, highlighting the most suitable bioindicators and providing essential insights into the factors that may influence ingestion rates. Additionally, the detection of PAEs in all species indicates the need for further re search on the contamination sources, the effects of these chemicals on marine organisms, and the potential risks to human health through seafood consumption.