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A collaborative trial involving 16 participants from nine European countries was conducted within the NORMAN network in efforts to harmonise suspect and non-target screening of environmental contaminants in whole fish samples of bream (Abramis brama). Participants were provided with freeze-dried, homogenised fish samples from a contaminated and a reference site, extracts (spiked and non-spiked) and reference sample preparation protocols for liquid chromatography (LC) and gas chromatography (GC) coupled to high resolution mass spectrometry (HRMS). Participants extracted fish samples using their in-house sample preparation method and/or the protocol provided. Participants correctly identified 9–69 % of spiked compounds using LC-HRMS and 20–60 % of spiked compounds using GC-HRMS. From the contaminated site, suspect screening with participants’ own suspect lists led to putative identification of on average ∼145 and ∼20 unique features per participant using LC-HRMS and GC-HRMS, respectively, while non-target screening identified on average ∼42 and ∼56 unique features per participant using LC-HRMS and GC-HRMS, respectively. Within the same sub-group of sample preparation method, only a few features were identified by at least two participants in suspect screening (16 features using LC-HRMS, 0 features using GC-HRMS) and non-target screening (0 features using LC-HRMS, 2 features using GC-HRMS). The compounds identified had log octanol/water partition coefficient (KOW) values from −9.9 to 16 and mass-to-charge ratios (m/z) of 68 to 761 (LC-HRMS and GC-HRMS). A significant linear trend was found between log KOW and m/z for the GC-HRMS data. Overall, these findings indicate that differences in screening results are mainly due to the data analysis workflows used by different participants. Further work is needed to harmonise the results obtained when applying suspect and non-target screening approaches to environmental biota samples.

The Watch List (WL) is a monitoring program under the European Water Framework Directive (WFD) to obtain high-quality Union-wide monitoring data on potential water pollutants for which scarce monitoring data or data of insufficient quality are available. The main purpose of the WL data collection is to determine if the substances pose a risk to the aquatic environment at EU level and subsequently to decide whether a threshold, the Environmental Quality Standards (EQS) should be set for them and, potentially to be listed as priority substance in the WFD. The first WL was established in 2015 and contained 10 individual or groups of substances while the 4th WL was launched in 2022. The results of monitoring the substances of the first WL showed that some countries had difficulties to reach an analytical Limit of Quantification (LOQ) below or equal to the Predicted No-Effect Concentrations (PNEC) or EQS. The Joint Research Centre (JRC) of the European Commission (EC) organised a series of workshops to support the EU Member States (MS) and their activities under the WFD. Sharing the knowledge among the Member States on the analytical methods is important to deliver good data quality. The outcome and the discussion engaged with the experts are described in this paper, and in addition a literature review of the most important publications on the analysis of 17-alpha-ethinylestradiol (EE2), amoxicillin, ciprofloxacin, metaflumizone, fipronil, metformin, and guanylurea from the last years is presented.

Chemicals infiltrate our daily experiences through multiple exposure pathways. Human biomonitoring (HBM) is routinely used to comprehensively understand these chemical interactions. Historically, HBM depended on targeted screening methods limited to a relatively small set of chemicals with triple quadrupole instruments typically. However, recent advances in high-resolution mass spectrometry (HRMS) have facilitated the use of broad-scope target, suspect, and non-target strategies, enhancing chemical exposome characterization within acceptable detection limits. Despite these advancements, establishing robust and efficient sample treatment protocols is still essential for trustworthy broad-range chemical analysis. This study sought to validate a methodology leveraging HRMS-based strategies for accurate profiling of exogenous chemicals and related metabolites in urine samples. We evaluated five extraction protocols, each encompassing various chemical classes, such as pharmaceuticals, plastic additives, personal care products, and pesticides, in terms of their extraction recoveries, linearity, matrix effect, sensitivity, and reproducibility. The most effective protocol was extensively validated and subsequently applied to 10 real human urine samples using wide-scope target analysis encompassing over 2000 chemicals. We successfully identified and semi-quantified a total of 36 chemicals using an ionization efficiency-based model, affirming the methodology's robust performance. Notably, our results dismissed the need for a deconjugation step, a typically labor-intensive and time-consuming process.

A collaborative trial involving 16 participants from nine European countries was conducted within the NORMAN network in efforts to harmonise suspect and non-target screening of environmental contaminants in whole fish samples of bream (Abramis brama). Participants were provided with freeze-dried, homogenised fish samples from a contaminated and a reference site, extracts (spiked and non-spiked) and reference sample preparation protocols for liquid chromatography (LC) and gas chromatography (GC) coupled to high resolution mass spectrometry (HRMS). Participants extracted fish samples using their in-house sample preparation method and/or the protocol provided. Participants correctly identified 9-69 % of spiked compounds using LC-HRMS and 20-60 % of spiked compounds using GC-HRMS. From the contaminated site, suspect screening with participants' own suspect lists led to putative identification of on average ∼145 and ∼20 unique features per participant using LC-HRMS and GC-HRMS, respectively, while non-target screening identified on average ∼42 and ∼56 unique features per participant using LC-HRMS and GC-HRMS, respectively. Within the same sub-group of sample preparation method, only a few features were identified by at least two participants in suspect screening (16 features using LC-HRMS, 0 features using GC-HRMS) and non-target screening (0 features using LC-HRMS, 2 features using GC-HRMS). The compounds identified had log octanol/water partition coefficient (KOW) values from -9.9 to 16 and mass-to-charge ratios (m/z) of 68 to 761 (LC-HRMS and GC-HRMS). A significant linear trend was found between log KOW and m/z for the GC-HRMS data. Overall, these findings indicate that differences in screening results are mainly due to the data analysis workflows used by different participants. Further work is needed to harmonise the results obtained when applying suspect and non-target screening approaches to environmental biota samples.

A collaborative trial involving 16 participants from nine European countries was conducted within the NORMAN network in efforts to harmonise suspect and non-target screening of environmental contaminants in whole fish samples of bream (Abramis brama). Participants were provided with freeze-dried, homogenised fish samples from a contaminated and a reference site, extracts (spiked and non-spiked) and reference sample preparation protocols for liquid chromatography (LC) and gas chromatography (GC) coupled to high resolution mass spectrometry (HRMS). Participants extracted fish samples using their in-house sample preparation method and/or the protocol provided. Participants correctly identified 9–69 % of spiked compounds using LC-HRMS and 20–60 % of spiked compounds using GC-HRMS. From the contaminated site, suspect screening with participants’ own suspect lists led to putative identification of on average ~145 and ~20 unique features per participant using LC-HRMS and GC-HRMS, respectively, while non-target screening identified on average ~42 and ~56 unique features per participant using LC-HRMS and GC-HRMS, respectively. Within the same sub-group of sample preparation method, only a few features were identified by at least two participants in suspect screening (16 features using LC-HRMS, 0 features using GC-HRMS) and non-target screening (0 features using LC-HRMS, 2 features using GC-HRMS). The compounds identified had log octanol/water partition coefficient (KOW) values from − 9.9 to 16 and mass-to-charge ratios (m/z) of 68 to 761 (LC-HRMS and GC-HRMS). A significant linear trend was found between log KOW and m/z for the GC-HRMS data. Overall, these findings indicate that differences in screening results are mainly due to the data analysis workflows used by different participants. Further work is needed to harmonise the results obtained when applying suspect and non-target screening approaches to environmental biota samples.

Syftet med den här studien var att studera förekomst av persistenta, mobila organiska miljöföroreningar (PMOC) i svensk vattenmiljö med fokus på risk för förorening av dricksvatten. Kända punktkällor och råvatten för dricksvattenproduktion i Mälarens närområde provtogs och analyserades med hjälp av högupplöst masspektrometeri (HRMS). Avrinning från flygplatser (n = 2), dagvatten (n = 7), lakvatten från deponier (n = 9) avloppsvatten från reningsverk (n = 15) och råvatten för dricksvattenproduktion (n = 3) ingick i studien och analyserades med metoder speciellt anpassade för mobila (polära) ämnen. Screeningen utgick från listor av tänkbara föroreningar som tagits fram genom in silico metoder och omfattade totalt 249 ämnen. Åtta PMOCs bekräftades och 24 identifierades (preliminärt) i vatten från punktkällor och/eller dricksvatten. Varje (preliminärt) identifierad substans som upptäcktes i råvatten återfanns även i flera typer av de påverkade miljöproverna (punktkällorna). De (preliminärt) identifierade substanserna bör undersökas vidare med avseende på ursprung och förekomst i miljön samt bedömas utifrån potentiella risker för miljön och som föroreningar i dricksvatten.

Återanvändning av avloppsvatten för jordbruksbevattning är ett sätt att minska efterfrågan på sötvatten, men det kan också introducera läkemedel, personliga hygienprodukter och andra kemikalier i jordbrukets ekosystem och livsmedelskedja. Syftet med denna studie var att mäta förekomsten av en rad potentiellt skadliga organiska mikroföroreningar (OMP), såsom läkemedel, personliga hygienprodukter, industrikemikalier, bekämpningsmedel och per- och polyfluoralkylsubstanser (PFAS) i avloppsvatten som används för bevattning och i den mottagande jordbruksmarken. Bevattningsvatten bestående av renat avloppsvatten vid två anläggningar på Gotland provtogs vid fyra tillfällen under juli och augusti 2021. Dessutom togs prover på jord och daggmaskar i september 2021 efter skörd från två åkrar bevattnade med avloppsvattnet samt från en åker som inte hade bevattnats alls. Potatis som fortfarande var i marken togs från ett av de bevattnade fälten. Ett brett spektrum av OMP-koncentrationer (ng/l till ug/l) hittades i bevattningsvattnet, och totalt upptäcktes 35 av 77 analyserade OMP. Totalt 19 av 24 olika PFAS detekterades i bevattningsvattnet i intervallet 0,1-1000 ng/l. Extraherbart organiskt fluor (EOF) och totala oxiderbara prekursorer (TOP) mättes även i vattenproverna. Intervallet för EOF var 366-507 ng/l och endast två av totalt åtta bevattningsvattenprover visade en liten ökning av perfluoroktansyra (PFOA) och perfluorhexansyra (PFHxA) efter oxidation. Ingen av OMP:erna i denna studie upptäcktes i något av jordproverna. Perfluoroktansulfonsyra (PFOS) hittades över detektionsgränsen i jord från båda bevattnade fälten (0,14-0,17 ng/ d.w.) men låg under detektionsgränsen i jord från referensplatsen. Perfluorbutansyra (PFBA) hittades i låga nivåer men över detektionsgränsen i ett av de bevattnade fälten (0,22 ng/g d.w.) och den närliggande referensplatsen (0,27 ng/g d.w.). EOF-analysen av jord resulterade inte i någon ytterligare information då detektionsgränsen var relativt hög, The reuse of wastewater for agricultural irrigation is one way to reduce the demand for freshwater but it can also introduce pharmaceuticals, personal care products, and other chemicals into the agricultural ecosystem and food chain. The aim of this study was to measure a range of potentially harmful organic micropollutants (OMPs), such as pharmaceuticals, personal care products, industrial chemicals, pesticides, and per- and polyfluoroalkyl substances (PFAS), in wastewater effluent used for irrigation and in the receiving farmland. Four sampling occasions of effluent water at two wastewater treatment plants in Gotland were conducted during July and August 2021. In addition, soil and earthworms were sampled in September 2021 after harvest from two fields irrigated with the monitored wastewater and one field that had not been irrigated that season. Potatoes still in the ground were sampled from one of the irrigated fields. A wide range of OMP concentrations (ng/L to ug/L) were found in the effluent water, and in total 35 of 77 analyzed OMPs were detected. A total of 19 out of 24 different PFAS were detected in the effluent samples in the range of 0.1-1000 ng/L. Extractable organofluorine (EOF) and total oxidizable precursors (TOP) were measured in water samples in addition to target PFAS. The range for EOF in effluent samples were 366-507 ng/L and only two samples out of the total eight effluent samples showed a small increase in concentrations of perfluorooctanoic acid (PFOA) and perfluorohexanoic acid (PFHxA) after oxidation. None of the OMPs in this study was detected in any of the soil samples. Perfluorooctane sulfonic acid (PFOS) was found over the detection limit in soil from both irrigated fields (0.14-0.17 ng/g d.w.) but was below the detection limit at the reference site. Perfluorobutanoic acid (PFBA) was found at low levels closely above the detection limit in one of the irrigated fields (0.22 ng/g d.w.) and the nearby reference site (0.27 ng/g d.w.). The E

TIMFIE (Time Integrating, Micro Flow, In situ Extraction) är en enkel och billig tidsintegrerad provtagningsmetod som här användes för bestämning av ett stort antal organiska ämnen från vitt skilda substansgrupper. Tekniken bygger på kontinuerlig fastfasextraktion i fält under en till två veckor och den efterföljande bestämningen av organiska ämnen är kvantitativ och baseras på helvatten, dvs. med partikelbunden fraktion inkluderad.Förutom organiska ämnen som växtskyddsmedel, PFAS och läkemedel mättes i detta projekt även metallhalter och löst organiskt kol (DOC) i det uppsamlade, filtrerade vattnet. Merparten av de studerade metallerna och DOC påverkades dock negativt av fastfaskolonnerna som används för extraktion av de organiska ämnena. En separat TIMFIE utan kolonner ska därför användas vid bestämning av metaller. En fältstudie med veckovisa TIMFIE-provtagningar i tolv provpunkter fördelade på fem regioner utfördes i samarbete med länsstyrelserna i Gotland, Östergötland och Dalarna samt med en avfallsanläggning i Mälardalen. Totalt analyserades 47 TIMFIE-prover för drygt 200 organiska ämnen och 21 metaller, samt ytterligare 8 TIMFIE-prover endast för metaller.I framtiden kommer två olika TIMFIE-provtagare att användas i studier där både organiska och oorganiska ämnen bestäms. Fortsatt arbete med att även inkludera näringsämnen i det oorganiska analyspaketet pågår och möjligheten att göra dessa bestämningar på ett återskapat helvatten undersöks.

The Spanish Mediterranean basin is particularly susceptible to climate change and human activities, making it vulnerable to the influence of anthropogenic contaminants. Therefore, conducting comprehensive and exhaustive water quality assessment in relevant water bodies of this basin is pivotal. In this work, surface water samples from coastal lagoons or estuaries were collected across the Spanish Mediterranean coastline and subjected to target and suspect screening of 1,585 organic micropollutants by liquid chromatography coupled to ion mobility separation and high resolution mass spectrometry. In total, 91 organic micropollutants could be confirmed and 5 were tentatively identified, with pharmaceuticals and pesticides being the most prevalent groups of chemicals. Chemical analysis data was compared with data on bioanalysis of those samples (recurrent aryl hydrocarbon receptor (AhR) activation, and estrogenic receptor (ER) inhibition in wetland samples affected by wastewater streams). The number of identified organic contaminants containing aromatic rings could explain the AhR activation observed. For the ER antagonistic effects, predictions on estrogenic inhibition potency for the detected compounds were used to explain the activities observed. The integration of chemical analysis with bioanalytical observations allowed a comprehensive overview of the quality of the water bodies under study.