Microplastic fibres (MPFs) often make up the largest fraction of microplastic pollution in aquatic environments, yet little is known about their degradative fate and persistence. This study investigates the environmentally relevant photodegradation of common MPFs: polyester (PET), polyamide (PA) and polyacrylonitrile (PAN), their respective additive chemical profile, together with their potential for additive leaching. MPFs were subject to ultraviolet (UV) exposure in seawater and freshwater media over 10 months. PET and PA MPFs showed significant fragmentation and surface changes following UV exposure, additionally PA showed evidence of chemical changes. PAN did not undergo significant photodegradation in the same exposure period. Chemicals tentatively identified in MPFs and aqueous leachates via non-target gas chromatography-mass spectrometry include monomers, UV stabilisers and degradation products. Characterisation of several bisphenols (BPs) and benzophenones (BzPs) was performed via ultraperformance liquid chromatography tandem mass spectrometry. Bisphenol A, bisphenol S and benzophenone-3 were quantified in all MPFs and wool at concentrations between 4.3 and 501 ng/g, with wool displaying the highest sum concentration of BPs and BzPs at 863 and 27 ng/g, respectively.

A rapid hybrid solid phase extraction (HybridSPE^®) protocol tailored to ultra-performance liquid chromatography–electrospray ionization tandem mass spectrometry (UPLC^®–ESI–MS/MS) analysis was developed for the determination of 15 per- and polyfluoroalkyl substances (PFAS) in liver tissue from harbour porpoises (Phocoena phocoena). The HybridSPE^® technique has been applied in trace concentration bioanalysis, but it was mainly used for liquid biological media until now. In this study, the protocol was applied on tissue matrix, and it demonstrated acceptable absolute recoveries (%) ranging from 44.4 to 89.4%. The chromatographic separation was carried out using a gradient elution program with a total run time of 4 min. The inter-day method precision ranged from 2.15 to 15.4%, and the method limits of detection (LODs) ranged from 0.003 to 0.30 ng/g wet weight (w.w.). A total of 20 liver samples were analyzed to demonstrate the applicability of the developed method in liver tissue from a wildlife species.

There is a growing concern about the occurrence of bisphenols and benzophenone UV filters in natural ecosystems, while data are limited regarding their actual occurrence in wildlife species, especially in raptors. In this study, concentrations of bisphenol and benzophenone UV filter analogues were determined in liver tissue samples (n = 38) from white-tailed eagles (Haliaeetus albicilla) that were found dead in Smøla (2006–2018), which is a Norwegian municipality that holds one of the densest breeding populations of white-tailed eagles in Europe. Bisphenol AF (BPAF; a fluorinated analogue) was the most ubiquitous contaminant since it was detected in 32 liver samples at concentrations ranging from 1.08 to 6.68 ng/g wet weight (w.w.), followed by bisphenol A (BPA, mean 10.4 ng/g w.w.), benzophenone-1 (BzP-1, mean 3.24 ng/g w.w.), and 4-hydroxybenzophenone (4-OH-BzP, mean 0.62 ng/g w.w.). The concentrations found in livers suggested that white-tailed eagles potentially accumulate bisphenols and benzophenone UV filters, which raises concern, as these plastic and personal care product-related emerging contaminants can show endocrine-disrupting properties. The high detection frequency of the fluorinated BPAF warrants further attention as other fluorinated compounds have proven to be extremely persistent and potentially harmful to wildlife.

A rapid hybrid solid phase extraction (HybridSPE®) protocol tailored to liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) analysis, was developed for the determination of four thyroid hormones, L-Thyroxine (T₄), 3,3',5-triiodo-L-thyronine (T₃), 3,3',5'-triiodo-L-thyronine (rT₃) and 3,3'-diiodo-L-thyronine (T₂) in blood plasma from Glaucous gulls (Larus hyperboreus) and Baikal seals (Phoca sibirica). The use of target analyte specific ¹³C internal standards allowed quantification to be performed through the standard solvent calibration curves and alleviated the need to perform quantification with matrix match curves. The relative recoveries were 100.0-110.1 % for T₄, 99.1-102.2 % for T₃, 100.5-108.0 % for rT₃, and 100.5-104.6 % for T₂. The matrix effects ranged from -1.52 to -6.10 %, demonstrating minor signal suppression during analysis. The method intra-day precision (method repeatability, RSD %, N = 5, k = 1 day) and inter-day precision (method reproducibility, RSD %, N = 10, k = 2 days) at the 1 ng/mL concentration of fortification were 8.54-15.4 % and 15.4-24.8 %, respectively, indicating acceptable chromatographic peak stabilities for all target THs even at trace level concentrations. The method limit of detection (LOD) for T₄, T₃, rT₃ and T₂ was 0.17, 0.16, 0.30 and 0.17 ng/mL, respectively. The HybridSPE® protocol was simple and rapid (<1 min) upon application, while the HybridSPE® cartridge did not require (as in classical SPE cartridges) any additional equilibration nor conditioning step prior sample loading. A total of 46 blood plasma samples, 30 samples collected from Glaucous gulls and 16 samples collected from Baikal seals, were analyzed for thyroid hormones to demonstrate the applicability of the developed method in these wildlife species. The concentrations of T₄ and T₃ in blood plasma from the Glaucous gulls were 5.95-44.2 and 0.37-5.61 ng/mL, respectively, whereas those from Baikal seals were 3.57-46.5 and 0.45-2.07 ng/mL, respectively. In both species, rT₃ demonstrated low detection rate, while T₂ was not detected. Furthermore, cross-array comparison between the HybridSPE®-LC-MS/MS protocol and an established routine radioimmunoassay (RIA) kit-based method was performed for T₄ and T₃ concentrations from selected Baikal seal plasma samples.