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AbstractThe Joint Research Centre (JRC) of the European Commission has recently released two new Certified Reference Materials (CRMs) for the analysis of brominated flame retardants (BFRs): the freshwater sediment ERM-CC537a and the fish tissue ERM-CE102. The production of these CRMs responds to the need of expanding the offer of quality assurance/quality control tools for the analysis of BFRs in the fields of environmental analysis and food control, especially for compliance purposes. The sediment ERM-CC537a carries certified values for polybrominated diphenyl ethers (PBDEs) and hexabromocyclododecane (HBCDD) diastereoisomers in the μg/kg range (dry mass), while the fish tissue ERM-CE102 is certified for PBDEs in the ng/kg range (wet weight). ERM-CC537a is the first reference material ever available with certified values for α-, β- and γ-HBCDD. The assignment of the certified values was performed via an intercomparison of expert laboratories. The evaluation of the data confirms the improving trend, observed in recent years, regarding the comparability of PBDE measurement results. The relative standard deviation (RSD) among laboratories is slightly better for the fish material (8–11%) compared to the sediment (9–15%), despite lower mass fractions in the biota matrix. The RSD of HBCDD data (17%) reveals that they are more challenging analytes. The average measurement uncertainty declared by the participants is about 30%, but an in-depth analysis of their performance reveals that it should be feasible to reduce the uncertainty budget.

In the past 12 years several studies have screened lists of thousands of chemicals available in the in-dustrial chemical inventories of the European Union, the USA and Canada with the goal of identifying andprioritizing chemicals which are persistent (P), bioaccumulative (B) and toxic (T). Most studies haveselected chemicals based on whether their predicted P and B properties and their long-range transportpotential exceed guideline thresholds for evaluation of persistent organic pollutants (POPs). A major goalof this study was to review this recent literature on computer-based or'in silico'screening for POPs. Asecond goal was to review other approaches forfinding previously unidentified chemicals of concernincluding targeted and non-target analytical approaches that might use lists of suspect chemicalsdeveloped from'in silico'screening studies. Eight studies were reviewed along with several others whichexamined the screening process and its uncertainties. From these studies we assembled a list of 3421chemicals, after removing duplicates and substances already on the Stockholm Convention on POPs.About 52% of these were halogenated, while 48% consisted of a broad range of non-halogenated organics.This list was then further analysed by calculating an overall"POPs score"for transport and accumulationin the Arctic for each substance using predicted partition coefficients, overall persistence, transfer effi-ciency, and bioaccumulation factor. A shorter list of twenty-five substances was developed based on theirPOPs score ranking. These substances had not been previously analysed in environmental media butwere nevertheless on current or recent chemical inventories indicating significant commercial use.

Abstract The aim of this paper is to present the conceptual framework for a Danish human biomonitoring (HBM) program. The EU and national science-policy interface, that is fundamental for a realization of the national and European environment and human health strategies, is discussed, including the need for a structured and integrated environmental and human health surveillance program at national level. In Denmark, the initiative to implement such activities has been taken. The proposed framework of the Danish monitoring program constitutes four scientific expert groups, i.e. i. Prioritization of the strategy for the monitoring program, ii. Collection of human samples, iii. Analysis and data management and iv. Dissemination of results produced within the program. This paper presents the overall framework for data requirements and information flow in the integrated environment and health surveillance program. The added value of an HBM program, and in this respect the objectives of national and European HBM programs supporting environmental health integrated policy-decisions and human health targeted policies, are discussed. In Denmark environmental monitoring has been prioritized by extensive surveillance systems of pollution in oceans, lakes and soil as well as ground and drinking water. Human biomonitoring has only taken place in research programs and few incidences of e.g. lead contamination. However an arctic program for HBM has been in force for decades and from the preparations of the EU-pilot project on HBM increasing political interest in a Danish program has developed.

Human biomonitoring is a powerful approach in assessing exposure to environmental pollutants. Flame retardants (FRs) are of particular concern due to their wide distribution in the environment and adverse health effects. This article reviews studies published in 2009-2020 on the chemical analysis of FRs in a variety of human samples and discusses the characteristics of the analytical methods applied to different FR biomarkers of exposure, including polybrominated diphenyl ethers (PBDEs), hexabromocyclododecane (HBCD), novel halogenated flame retardants (NHFRs), bromophenols, incl. tetrabromobisphenol A (TBBPA), and organophosphorous flame retardants (PFRs). Among the extraction techniques, liquid-liquid extraction (LLE) and solid phase extraction (SPE) were used most frequently due to the good efficiencies in the isolation of the majority of the FR biomarkers, but with challenges for highly lipophilic FRs. Gas chromatography-mass spectrometry (GC-MS) is mainly applied in the instrumental analysis of PBDEs and most NHFRs, with recent inclusions of GC-MS/MS and high resolution MS techniques. Liquid chromatography-MS/MS is mainly applied to HBCD, bromophenols, incl. TBBPA, and PFRs (including metabolites), however, GC-based analysis following derivatization has also been used for phenolic compounds and PFR metabolites. Developments are noticed towards more universal analytical methods, which enable widening method scopes in the human biomonitoring of FRs. Challenges exist with regard to sensitivity required for the low concentrations of FRs in the general population and limited sample material for some human matrices. A strong focus on quality assurance/quality control (QA/QC) measures is required in the analysis of FR biomarkers in human samples, related to their variety of physical-chemical properties, low levels in most human samples and the risk of contamination. ; This study was part of the HBM4EU project receiving funding from the European Union's Horizon 2020 research and innovation programme under Grant ...

The Human Biomonitoring for Europe initiative (HBM4EU) aims to study the exposure of citizens to chemicals and potentially associated health effects. One objective of this project has been to build a network of laboratories able to answer to the requirements of European human biomonitoring studies. Within the HBM4EU quality assurance and quality control scheme (QA/QC), a number of interlaboratory comparison investigations (ICIs) and external quality assurance schemes (EQUASs) were organized to ensure data consistency, comparability and reliability. Bisphenols are among the prioritized substance groups in HBM4EU, including bisphenol A (BPA), bisphenol S (BPS) and bisphenol F (BPF) in human urine. In four rounds of ICI/EQUAS, two target concentration levels were considered, related to around P25 and P95 of the typical exposure distribution observed in the European general population. Special attention was paid to the conjugated phase II metabolites known to be most dominant in samples of environmentally exposed individuals, through the analysis of both native samples and samples fortified with glucuronide forms. For the low level, the average percentage of satisfactory results across the four rounds was 83% for BPA, 71% for BPS and 62% for BPF. For the high level, the percentages of satisfactory results increased to 93% for BPA, 89% for BPS and 86% for BPF. 24 out of 32 participating laboratories (75%) were approved for the analyses of BPA in the HBM4EU project according to the defined criterion of Z-scores for both low and high concentration levels in at least two ICI/EQUAS rounds. For BPS and BPF, the number of qualified laboratories was 18 out of 27 (67%) and 13 out of 28 (46%), respectively. These results demonstrate a strong analytical capability for BPA and BPS in Europe, while improvements may be needed for BPF. ; We gratefully acknowledge funding by the European Union's Horizon 2020 research and innovation programme under the grant agreement No. 733032 HBM4EU. The authors would like to thank the HBM4EU ...

A quality assurance/quality control program was implemented in the framework of the EU project HBM4EU to assess and improve the comparability of biomarker analysis and to build a network of competent laboratories. Four rounds of proficiency tests were organized for 15 phthalate and two DINCH urinary biomarkers (0.2-138 ng/mL) over a period of 18 months, with the involvement of 28 laboratories. A substantial improvement in performance was observed after the first round in particular, and by the end of the program, an average satisfactory performance rate of 90% was achieved. The interlaboratory reproducibility as derived from the participants' results varied for the various biomarkers and rounds, with an average of 24% for the biomarkers of eight single-isomer phthalates (e.g., DnBP and DEHP) and 43% for the more challenging biomarkers of the mixed-isomer phthalates (DiNP, DiDP) and DINCH. When the reproducibility was based only on the laboratories that consistently achieved a satisfactory performance, this improved to 17% and 26%, respectively, clearly demonstrating the success of the QA/QC efforts. The program thus aided in building capacity and the establishment of a network of competent laboratories able to generate comparable and accurate HBM data for phthalate and DINCH biomarkers in 14 EU countries. In addition, global comparability was ensured by including external expert laboratories. ; This study was part of the HBM4EU project receiving funding from the European Union's Horizon 2020 research and innovation program under grant agreement No 733032. Co-funding was received from the Dutch Ministry of Agriculture, Nature and Food Quality (project KB 37-002-014-001/002). ; Sí

The major purpose of human biomonitoring is the mapping and assessment of human exposure to chemicals. The European initiative HBM4EU has prioritized seven substance groups and two metals relevant for human exposure: Phthalates and substitutes (1,2-cyclohexane dicarboxylic acid diisononyl ester, DINCH), bisphenols, per- and polyfluoroalkyl substances (PFASs), halogenated and organophosphorous flame retardants (HFRs and OPFRs), polycyclic aromatic hydrocarbons (PAHs), arylamines, cadmium and chromium. As a first step towards comparable European-wide data, the most suitable biomarkers, human matrices and analytical methods for each substance group or metal were selected from the scientific literature, based on a set of selection criteria. The biomarkers included parent compounds of PFASs and HFRs in serum, of bisphenols and arylamines in urine, metabolites of phthalates, DINCH, OPFRs and PAHs in urine as well as metals in blood and urine, with a preference to measure Cr in erythrocytes representing Cr (VI) exposure. High performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) was the method of choice for bisphenols, PFASs, the HFR hexabromocyclododecane (HBCDD), phenolic HFRs as well as the metabolites of phthalates, DINCH, OPFRs and PAHs in urine. Gas chromatographic (GC) methods were selected for the remaining compounds, e.g. GC-low resolution MS with electron capture negative ionization (ECNI) for HFRs. Both GC-MS and LC-MS/MS were suitable for arylamines. New developments towards increased applications of GC-MS/MS may offer alternatives to GC-MS or LC-MS/MS approaches, e.g. for bisphenols. The metals were best determined by inductively coupled plasma (ICP)-MS, with the particular challenge of avoiding interferences in the Cd determination in urine. The evaluation process revealed research needs towards higher sensitivity and non-invasive sampling as well as a need for more stringent quality assurance/quality control applications and assessments. ; This study was part of the HBM4EU project receiving funding from the European Union's Horizon 2020 research and innovation programme under grant agreement No 733032. The authors acknowledge Ana Gonzalez Antuña (University of Las Palmas de Gran Canaria), Lauma Buša (University of Latvia), Govindan Malarvannan and Celine Gys (University of Antwerp) for their help with the literature search. ; Sí

A fundamental objective of the human biomonitoring for Europe initiative (HBM4EU) is to progress toward comparable and robust exposure data for a wide variety of prioritized chemicals in human samples. A programme for Quality Assurance/Quality Control (QA/QC) was designed in HBM4EU with the purpose of creating a network of European laboratories providing comparable analytical data of high quality. Two approaches were chosen for two sets of prioritized chemicals with different timelines: (i) Scheme 1, where interested candidate laboratories participated in multiple rounds of proficiency tests (ii) Scheme 2, where selected expert laboratories participated in three rounds of interlaboratory comparison investigations. In both cases, the results were used to identify laboratories capable of generating consistent and comparable results for sample analysis in the frame of HBM4EU. In total, 84 laboratories from 26 countries were invited to participate in Scheme 1 that covered up to 73 biomarkers from Hexamoll® DINCH, phthalates, bisphenols, per- and polyfluoroalkyl substances, halogenated flame retardants (HFRs), organophosporous flame retardants (OPFRs), polycyclic aromatic hydrocarbons (PAH), cadmium, chromium and aromatic amines. 74 of the participants were successful for at least one biomarker in Scheme 1. Scheme 2 involved 22 biomarkers and successful results were obtained by 2 expert laboratories for arsenic, 5 for acrylamide, 4 for mycotoxins, 2 for pesticides and 2 for UV-filters in skin care products. The QA/QC programme allowed the identification of major difficulties and needs in HBM analysis as well of gaining insight in the analytical capacities of European laboratories. Furthermore, it is the first step towards the establishment of a sustainable European network of HBM laboratories. ; This study was part of the HBM4EU project receiving funding from the European Union's Horizon 2020 research and innovation programme under grant agreement No 733032. The authors acknowledge all the participating and expert laboratories (Centre de Toxicologie du Québec/Institut National de Santé Publique du Québec; IDEA Consultants, Inc.; Otsuka Pharmaceutical Co., Ltd.; Otsuka Pharmaceutical Co., Ltd.; Arizona Department of Health Services Laboratory; Centers for Disease Control and Prevention (CDC); New York State Department of Health Wadsworth Center; Wisconsin State Laboratory of Hygiene), that made the HBM4EU QA/QC programme possible, as well as the Management and Advisory Boards of HBM4EU. ; Sí

The European Human Biomonitoring Initiative (HBM4EU) is coordinating and advancing human biomonitoring (HBM). For this purpose, a network of laboratories delivering reliable analytical data on human exposure is fundamental. The analytical comparability and accuracy of laboratories analysing flame retardants (FRs) in serum and urine were investigated by a quality assurance/quality control (QA/QC) scheme comprising interlaboratory comparison investigations (ICIs) and external quality assurance schemes (EQUASs). This paper presents the evaluation process and discusses the results of four ICI/EQUAS rounds performed from 2018 to 2020 for the determination of ten halogenated flame retardants (HFRs) represented by three congeners of polybrominated diphenyl ethers (BDE-47, BDE-153 and BDE-209), two isomers of hexabromocyclododecane (α-HBCD and γ-HBCD), two dechloranes (anti-DP and syn-DP), tetrabromobisphenol A (TBBPA), decabromodiphenylethane (DBDPE), and 2,4,6-tribromophenol (2,4,6-TBP) in serum, and four metabolites of organophosphorus flame retardants (OPFRs) in urine, at two concentration levels. The number of satisfactory results reported by laboratories increased during the four rounds. In the case of HFRs, the scope of the participating laboratories varied substantially (from two to ten) and in most cases did not cover the entire target spectrum of chemicals. The highest participation rate was reached for BDE-47 and BDE-153. The majority of participants achieved more than 70% satisfactory results for these two compounds over all rounds. For other HFRs, the percentage of successful laboratories varied from 44 to 100%. The evaluation of TBBPA, DBDPE, and 2,4,6-TBP was not possible because the number of participating laboratories was too small. Only seven laboratories participated in the ICI/EQUAS scheme for OPFR metabolites and five of them were successful for at least two biomarkers. Nevertheless, the evaluation of laboratory performance using Z-scores in the first three rounds required an alternative approach compared to HFRs because of the small number of participants and the high variability of experts' results. The obtained results within the ICI/EQUAS programme showed a significant core network of comparable European laboratories for HBM of BDE-47, BDE-153, BDE-209, α-HBCD, γ-HBCD, anti-DP, and syn-DP. On the other hand, the data revealed a critically low analytical capacity in Europe for HBM of TBBPA, DBDPE, and 2,4,6-TBP as well as for the OPFR biomarkers. ; We gratefully acknowledge funding by the European Union's Horizon 2020 research and innovation programme under the grant agreement No. 733032. ; Sí

The major purpose of human biomonitoring is the mapping and assessment of human exposure to chemicals. The European initiative HBM4EU has prioritized seven substance groups and two metals relevant for human exposure: Phthalates and substitutes (1,2-cyclohexane dicarboxylic acid diisononyl ester, DINCH), bisphenols, per- and polyfluoroalkyl substances (PFASs), halogenated and organophosphorous flame retardants (HFRs and OPFRs), polycyclic aromatic hydrocarbons (PAHs), arylamines, cadmium and chromium. As a first step towards comparable European-wide data, the most suitable biomarkers, human matrices and analytical methods for each substance group or metal were selected from the scientific literature, based on a set of selection criteria. The biomarkers included parent compounds of PFASs and HFRs in serum, of bisphenols and arylamines in urine, metabolites of phthalates, DINCH, OPFRs and PAHs in urine as well as metals in blood and urine, with a preference to measure Cr in erythrocytes representing Cr (VI) exposure. High performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) was the method of choice for bisphenols, PFASs, the HFR hexabromocyclododecane (HBCDD), phenolic HFRs as well as the metabolites of phthalates, DINCH, OPFRs and PAHs in urine. Gas chromatographic (GC) methods were selected for the remaining compounds, e.g. GC-low resolution MS with electron capture negative ionization (ECNI) for HFRs. Both GC–MS and LC-MS/MS were suitable for arylamines. New developments towards increased applications of GC–MS/MS may offer alternatives to GC–MS or LC-MS/MS approaches, e.g. for bisphenols. The metals were best determined by inductively coupled plasma (ICP)-MS, with the particular challenge of avoiding interferences in the Cd determination in urine. The evaluation process revealed research needs towards higher sensitivity and non-invasive sampling as well as a need for more stringent quality assurance/quality control applications and assessments. ; This study was part of the HBM4EU project receiving funding from the European Union's Horizon 2020 research and innovation programme under grant agreement No 733032.

We reviewed compliance monitoring requirements in the European Union, the United States, and the Oslo-Paris Convention for the protection of the marine environment of the North-East Atlantic, and evaluated if these are met by passive sampling methods for nonpolar compounds. The strengths and shortcomings of passive sampling are assessed for water, sediments, and biota. Passive water sampling is a suitable technique for measuring concentrations of freely dissolved compounds. This method yields results that are incompatible with the EU's quality standard definition in terms of total concentrations in water, but this definition has little scientific basis. Insufficient quality control is a present weakness of passive sampling in water. Laboratory performance studies and the development of standardized methods are needed to improve data quality and to encourage the use of passive sampling by commercial laboratories and monitoring agencies. Successful prediction of bioaccumulation based on passive sampling is well documented for organisms at the lower trophic levels, but requires more research for higher levels. Despite the existence of several knowledge gaps, passive sampling presently is the best available technology for chemical monitoring of nonpolar organic compounds. Key issues to be addressed by scientists and environmental managers are outlined.

Funding text 1 We would like to acknowledge all site and laboratory operators and students at all AMAP stations. Wong is grateful to Desmond Ng and Jared Chisamore of Environment and Climate Change Canada for help in data analysis. Financial support for the monitoring programmes was provided by the Northern Contaminants Program, Crown-Indigenous Relations and Northern Affairs Canada (Alert); Swedish-EPA (Naturv?rdsverket) and the Finnish Meteorological Institute (Pallas); the Icelandic Ministry for the Environment (St?rh?f?i); the Norwegian Environment Agency (Zeppelin and And?ya); and the Danish Environmental Protection Agency (Villum Research Station). RPA ?Typhoon?, Roshydromet provided support for air monitoring at sites in Russia (Amderma and Tiksi). The Government of Canada's Chemicals Management Plan (CMP) provided partial funding for the analysis of emerging contaminants at Alert. Funding text 2 We would like to acknowledge all site and laboratory operators and students at all AMAP stations. Wong is grateful to Desmond Ng and Jared Chisamore of Environment and Climate Change Canada for help in data analysis. Financial support for the monitoring programmes was provided by the Northern Contaminants Program, Crown-Indigenous Relations and Northern Affairs Canada (Alert); Swedish-EPA ( Naturvårdsverket ) and the Finnish Meteorological Institute (Pallas); the Icelandic Ministry for the Environment (Stórhöfði); the Norwegian Environment Agency (Zeppelin and Andøya); and the Danish Environmental Protection Agency (Villum Research Station). RPA 'Typhoon', Roshydromet provided support for air monitoring at sites in Russia (Amderma and Tiksi). The Government of Canada 's Chemicals Management Plan (CMP) provided partial funding for the analysis of emerging contaminants at Alert. Publisher Copyright: © 2021 ; The long-term time trends of atmospheric pollutants at eight Arctic monitoring stations are reported. The work was conducted under the Arctic Monitoring and Assessment Programme (AMAP) of the Arctic Council. ...

AbstractA large number of apex predator samples are available in European research collections, environmental specimen banks and natural history museums that could be used in chemical monitoring and regulation. Apex predators bioaccumulate pollutants and integrate contaminant exposure over large spatial and temporal scales, thus providing key information for risk assessments. Still, present assessment practices under the different European chemical legislations hardly use existing chemical monitoring data from top predators. Reasons include the lack of user-specific guidance and the fragmentation of data across time and space. The European LIFE APEX project used existing sample collections and applied state-of-the-art target and non-target screening methods, resulting in the detection of > 4,560 pollutants including legacy compounds. We recommend establishing infrastructures that include apex predators as an early warning system in Europe. Chemical data of apex species from freshwater, marine and terrestrial compartments should become an essential component in future chemical assessment and management across regulations, with the purpose to (1) validate registration data with 'real world' measurements and evaluate the predictability of current models; (2) identify and prioritise hazardous chemicals for further assessment; (3) use data on food web magnification as one line of evidence to assess biomagnification; (4) determine the presence of (bio)transformations products and typical chemical mixtures, and (5) evaluate the effectiveness of risk management measures by trend analysis. We highlight the achievements of LIFE APEX with regard to novel trend and mixture analysis tools and prioritisation schemes. The proposed advancements complement current premarketing regulatory assessments and will allow the detection of contaminants of emerging concern at an early stage, trigger risk management measures and evaluations of their effects with the ultimate goal to protect humans and the environment. This is the second policy brief of the LIFE APEX project.

AbstractMonitoring data from apex predators were key drivers in the development of early chemicals legislations due to the population declines of many species during the twentieth century, which was linked to certain persistent organic pollutants (POPs). Besides triggering the development of global treaties (e.g. the Stockholm Convention), chemical monitoring data from apex predators have been particularly important for identifying compounds with bioaccumulative properties under field conditions. Many apex predators are protected species and only a few environmental specimen banks (ESBs) regularly collect samples as many ESBs were established during the 1980–1990s when apex predators were scarce. Today, many POPs have been banned, which contributed to the recovery of many apex predator populations. As a consequence, apex predator samples are now available in research collections (RCs) and natural history museums (NHMs). These samples can be used for routine analysis as well as for screening studies using novel analytical techniques and advanced data treatment workflows, such as suspect and non-target screening. The LIFE APEX project has demonstrated how these samples can be used in a cost-efficient way to generate data on legacy compounds and contaminants of emerging concern. Furthermore, it has described quality assurance/control measures to ensure high quality and comparable data, with a view to uses in chemicals risk assessment and management. To increase the visibility of available sample collections and monitoring data from apex predators we developed accessible online database systems. Additionally, the acquired high-resolution mass spectrometric data were stored in a digital sample freezing platform that allows retrospective suspect screening in previously analysed samples for substances that may be of concern/under assessment in the future. These databases provide open access to a wide range of chemical data, for use by regulators, researchers, industry and the general public, and contribute to a stronger link between science and policy.