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      Fluorescence polarization immunoassay for the determination of diclofenac in wastewater

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          Abstract

          Pharmacologically active compounds are often detected in wastewater and surface waters. The nonsteroidal anti-inflammatory drug diclofenac (DCF) was included in the European watch list of substances that requires its environmental monitoring in the member states. DCF may harmfully influence the ecosystem already at concentrations ≤ 1 μg L −1. The fast and easy quantification of DCF is becoming a subject of global importance. Fluorescence polarization immunoassay (FPIA) is a homogeneous mix-and-read method which does not require the immobilization of reagents. FPIA can be performed in one phase within 20–30 min, making it possible to analyse wastewater without any complicated pre-treatment. In this study, new tracer molecules with different structures, linking fluorophores to derivatives of the analyte, were synthesized, three homologous tracers based on DCF, two including a C 6 spacer, and one heterologous tracer derived from 5-hydroxy-DCF. The tracer molecules were thoroughly assessed for performance. Regarding sensitivity of the FPIA, the lowest limit of detection reached was 2.0 μg L −1 with a working range up to 870 μg L −1. The method was validated for real wastewater samples against LC-MS/MS as reference method with good agreement of both methods.

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          Supplementary Information

          The online version contains supplementary material available at 10.1007/s00216-020-03058-w.

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          Most cited references31

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          EU-wide survey of polar organic persistent pollutants in European river waters.

          This study provides the first EU-wide reconnaissance of the occurrence of polar organic persistent pollutants in European river waters. More than 100 individual water samples from over 100 European rivers from 27 European Countries were analysed for 35 selected compounds, comprising pharmaceuticals, pesticides, PFOS, PFOA, benzotriazoles, hormones, and endocrine disrupters. Around 40 laboratories participated in this sampling exercise. The most frequently and at the highest concentration levels detected compounds were benzotriazole, caffeine, carbamazepine, tolyltriazole, and nonylphenoxy acetic acid (NPE(1)C). Only about 10% of the river water samples analysed could be classified as "very clean" in terms of chemical pollution. The rivers responsible for the major aqueous emissions of PFOS and PFOA from the European Continent could be identified. For the target compounds chosen, we are proposing "indicative warning levels" in surface waters, which are (for most compounds) close to the 90th percentile of all water samples analysed.
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            Fate of diclofenac in municipal wastewater treatment plant - a review.

            Diclofenac (DCF) is a common anti-inflammatory pharmaceutical that is often detected in waste wasters, effluents and surface waters. Recently, DCF was included in the watch list of substances in EU that requires its environmental monitoring in the member states. DCF is also known to harmfully affect several environmental species already at concentrations of ≤ 1 μg/l. This review focuses on the occurrence and fate of DCF in conventional wastewater treatment processes. Research done in this area was gathered and analyzed in order to find out the possibilities to enhance DCF elimination during biological wastewater treatment. More precisely, human metabolism, concentrations in wastewater influents and effluents, elimination rates in the treatment train, roles of sorption and biotransformation mechanisms during the treatment as well as formation of transformation products are reported. Additionally, the effect of process configuration, i.e. conventional activated sludge (CAS), biological nutrient removal (BNR), membrane bioreactor (MBR) and attached-growth bioreactor, and process parameters, i.e. solids retention time (SRT) and hydraulic retention time (HRT) are presented. Generally, DCF is poorly biodegradable which often translates into low elimination rates during biological wastewater treatment. Only a minor portion is sorbed to sludge. MBR and attached-growth bioreactors may result in higher elimination of DCF over CAS or BNR. Long SRTs (>150 d) favor the DCF elimination due to sludge adaptation. Longer HRTs (>2-3d) could significantly increase the elimination of DCF during biological wastewater treatment. Bioaugmentation could be used to enhance DCF elimination, however, this requires more research on microbial communities that are able to degrade DCF. Also, further research is needed to gain more information about the deconjugation processes and biotic and abiotic transformation and the nature of transformation products.
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              Liquid chromatography-tandem mass spectrometry for the analysis of pharmaceutical residues in environmental samples: a review.

              Pharmaceutical residues are environmental contaminants of recent concern and the requirements for analytical methods are mainly dictated by low concentrations found in aqueous and solid environmental samples. In the current article, a review of the liquid chromatography-tandem mass spectrometry (LC-MS/MS) based methods published so far for the determination of pharmaceuticals in the environment is presented. Pharmaceuticals included in this review are antibiotics, non-steroidal anti-inflammatory drugs, beta-blockers, lipid regulating agents and psychiatric drugs. Advanced aspects of current LC-MS/MS methodology, including sample preparation and matrix effects, are discussed.
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                Author and article information

                Contributors
                rudolf.schneider@bam.de
                Journal
                Anal Bioanal Chem
                Anal Bioanal Chem
                Analytical and Bioanalytical Chemistry
                Springer Berlin Heidelberg (Berlin/Heidelberg )
                1618-2642
                1618-2650
                25 November 2020
                25 November 2020
                2021
                : 413
                : 4
                : 999-1007
                Affiliations
                [1 ]GRID grid.71566.33, ISNI 0000 0004 0603 5458, Bundesanstalt für Materialforschung und -prüfung (BAM), ; 12200 Berlin, Germany
                [2 ]GRID grid.7468.d, ISNI 0000 0001 2248 7639, Department of Chemistry, , Humboldt-Universität zu Berlin, ; 10099 Berlin, Germany
                [3 ]GRID grid.14476.30, ISNI 0000 0001 2342 9668, Chemical Faculty, , M.V. Lomonosov Moscow State University, ; Moscow, Russian Federation 119991
                [4 ]GRID grid.6734.6, ISNI 0000 0001 2292 8254, Technische Universität Berlin, ; Straße des 17. Juni 135, 10623 Berlin, Germany
                Article
                3058
                10.1007/s00216-020-03058-w
                7813709
                33241445
                7d42ef08-23bd-4364-9863-59177af0d90d
                © The Author(s) 2020

                Open Access This article is licensed under a Creative Commons Attribution 4.0 International License, which permits use, sharing, adaptation, distribution and reproduction in any medium or format, as long as you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons licence, and indicate if changes were made. The images or other third party material in this article are included in the article's Creative Commons licence, unless indicated otherwise in a credit line to the material. If material is not included in the article's Creative Commons licence and your intended use is not permitted by statutory regulation or exceeds the permitted use, you will need to obtain permission directly from the copyright holder. To view a copy of this licence, visit http://creativecommons.org/licenses/by/4.0/.

                History
                : 5 February 2020
                : 8 November 2020
                : 10 November 2020
                Funding
                Funded by: FundRef http://dx.doi.org/10.13039/100009553, Bundesanstalt für Materialforschung und -Prüfung;
                Award ID: BAM MI1_2015_55
                Categories
                Research Paper
                Custom metadata
                © Springer-Verlag GmbH Germany, part of Springer Nature 2021

                Analytical chemistry
                diclofenac,fpia,water,wastewater,nsaid
                Analytical chemistry
                diclofenac, fpia, water, wastewater, nsaid

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