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      When every particle matters: A QuEChERS approach to extract microplastics from environmental samples

      research-article
      * , , , ,
      MethodsX
      Elsevier
      QuEChERS, Quick, Easy, Cheap, Effective, Rugged, Safe, MP, microplastics, μFTIR, micro Fourier transform infrared, ATR, attenuated total reflection, MPF, microplastic free, SPT, sodium polytungstate, QA, quality assurance, QC, quality control, PTFE, polytetrafluoroethylene, UR, user requirements, SR, system requirements, TS, technical solution, SI, supplementary information, MQ (water), MilliQ (water)/ ultrapure water, SOPs, standard operation procedures, A QuEChERS approach to extract microplastics from environmental samples, Sequential protocol, Purification technique, Chemical digestion, Handbook for laboratory work, Manual for good practices on microplastic extraction, Contamination prevention, Recovery rates, Wastewater, Particle-rich

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          Abstract

          The identification of microplastics (MP), especially small (<500 μm) MP, using automated surface-chemistry approaches requires the best possible reduction of natural particles whilst preserving the integrity of the targeted synthetic polymers particles. In general, both natural and synthetic particles can be highly diverse physically and chemically and MP extraction, particularly from complex matrices such as sediments, sludge and soils, requires efficient method pipelines. Our paper presents a universal framework of modular protocols (presented in a decision tree) that fulfil predefined user requirements (QuEChERS: Quick, Easy, Cheap, Effective, Rugged, Safe) as well as providing best practises for reasonable MP working conditions within a standard laboratory. New procedures and technical innovations for density separation of particle-rich matrices are presented, such as a spiral conveyor developed and validated for MP recovery. In sharing such best-practice protocols, we aim to help in the push towards MP quantification method standardisation.

          • Publication of protocols of an entire MP extraction (10 μm – 5 mm) pipeline for particle-based analysis of various environmental matrices

          • Modularity: Optimised quantitative sample preparation adapted to particle sizes and sample matrices

          • New protocols and technical innovations (e.g. spiral conveyor) optimise MP extraction

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          Most cited references22

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          Isolation of microplastics in biota-rich seawater samples and marine organisms

          Microplastic litter is a pervasive pollutant present in aquatic systems across the globe. A range of marine organisms have the capacity to ingest microplastics, resulting in adverse health effects. Developing methods to accurately quantify microplastics in productive marine waters, and those internalized by marine organisms, is of growing importance. Here we investigate the efficacy of using acid, alkaline and enzymatic digestion techniques in mineralizing biological material from marine surface trawls to reveal any microplastics present. Our optimized enzymatic protocol can digest >97% (by weight) of the material present in plankton-rich seawater samples without destroying any microplastic debris present. In applying the method to replicate marine samples from the western English Channel, we identified 0.27 microplastics m−3. The protocol was further used to extract microplastics ingested by marine zooplankton under laboratory conditions. Our findings illustrate that enzymatic digestion can aid the detection of microplastic debris within seawater samples and marine biota.
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            Sampling, isolating and identifying microplastics ingested by fish and invertebrates

            Microplastic debris (<5 mm) is a prolific environmental pollutant, found worldwide in marine, freshwater and terrestrial ecosystems. This review assesses the numerous different methods used to identify microplastics ingested by marine organisms. Microplastic debris (<5 mm) is a prolific environmental pollutant, found worldwide in marine, freshwater and terrestrial ecosystems. Interactions between biota and microplastics are prevalent, and there is growing evidence that microplastics can incite significant health effects in exposed organisms. To date, the methods used to quantify such interactions have varied greatly between studies. Here, we critically review methods for sampling, isolating and identifying microplastics ingested by environmentally and laboratory exposed fish and invertebrates. We aim to draw attention to the strengths and weaknesses of the suite of published microplastic extraction and enumeration techniques. Firstly, we highlight the risk of microplastic losses and accumulation during biotic sampling and storage, and suggest protocols for mitigating contamination in the field and laboratory. We evaluate a suite of methods for extracting microplastics ingested by biota, including dissection, depuration, digestion and density separation. Lastly, we consider the applicability of visual identification and chemical analyses in categorising microplastics. We discuss the urgent need for the standardisation of protocols to promote consistency in data collection and analysis. Harmonized methods will allow for more accurate assessment of the impacts and risks microplastics pose to biota and increase comparability between studies.
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              Validation of a Method for Extracting Microplastics from Complex, Organic-Rich, Environmental Matrices

              Complex and organic-rich solid substrates such as sludge and soil have been shown to be contaminated by microplastics; however, methods for extracting plastic particles have not yet been systemically tested or standardized. This study investigated four main protocols for the removal of organic material during analysis of microplastics from complex solid matrices: oxidation using H2O2, Fenton's reagent, and alkaline digestion with NaOH and KOH. Eight common polymer types were used to assess the influence of reagent exposure on particle integrity. Organic matter removal efficiencies were established for test sludge and soil samples. Fenton's reagent was identified as the optimum protocol. All other methods showed signs of particle degradation or resulted in an insufficient reduction in organic matter content. A further validation procedure revealed high microplastic extraction efficiencies for particles with different morphologies. This confirmed the suitability of Fenton's reagent for use in conjunction with density separation for extracting microplastics. This approach affords greater comparability with existing studies that utilize a density-based technique. Recommendations for further method optimization were also identified to improve the recovery of microplastic from complex, organic-rich environmental samples.
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                Author and article information

                Contributors
                Journal
                MethodsX
                MethodsX
                MethodsX
                Elsevier
                2215-0161
                15 January 2020
                2020
                15 January 2020
                : 7
                : 100784
                Affiliations
                [0005]Leibniz Institute for Baltic Sea Research, Seestraße 15, 18119 Rostock, Germany
                Author notes
                Article
                S2215-0161(20)30004-2 100784
                10.1016/j.mex.2020.100784
                7016028
                f745ec47-0a0d-449b-96b8-2eab45be479d
                © 2020 Published by Elsevier B.V.

                This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

                History
                : 30 December 2019
                Categories
                Article(s) from the Special Issue on Microplastics analysis

                quechers, quick, easy, cheap, effective, rugged, safe,mp, microplastics,μftir, micro fourier transform infrared,atr, attenuated total reflection,mpf, microplastic free,spt, sodium polytungstate,qa, quality assurance,qc, quality control,ptfe, polytetrafluoroethylene,ur, user requirements,sr, system requirements,ts, technical solution,si, supplementary information,mq (water), milliq (water)/ ultrapure water,sops, standard operation procedures,a quechers approach to extract microplastics from environmental samples,sequential protocol,purification technique,chemical digestion,handbook for laboratory work,manual for good practices on microplastic extraction,contamination prevention,recovery rates,wastewater,particle-rich

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