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Optimization, performance, and application of a pyrolysis-GC/MS method for the identification of microplastics

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Abstract

Plastics are found to be major debris composing marine litter; microplastics (MP, < 5 mm) are found in all marine compartments. The amount of MPs tends to increase with decreasing size leading to a potential misidentification when only visual identification is performed. These last years, pyrolysis coupled with gas chromatography/mass spectrometry (Py-GC/MS) has been used to get information on the composition of polymers with some applications on MP identification. The purpose of this work was to optimize and then validate a Py-GC/MS method, determine limit of detection (LOD) for eight common polymers, and apply this method on environmental MP. Optimization on multiple GC parameters was carried out using polyethylene (PE) and polystyrene (PS) microspheres. The optimized Py-GC/MS method require a pyrolysis temperature of 700 °C, a split ratio of 5 and 300 °C as injector temperature. Performance assessment was accomplished by performing repeatability and intermediate precision tests and calculating limit of detection (LOD) for common polymers. LODs were all below 1 μg. For performance assessment, identification remains accurate despite a decrease in signal over time. A comparison between identifications performed with Raman micro spectroscopy and with Py-GC/MS was assessed. Finally, the optimized method was applied to environmental samples, including plastics isolated from sea water surface, beach sediments, and organisms collected in the marine environment. The present method is complementary to μ-Raman spectroscopy as Py-GC/MS identified pigment containing particles as plastic. Moreover, some fibers and all particles from sediment and sea surface were identified as plastic.

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Acknowledgments

Ludovic Hermabessiere is grateful to the Hauts-de-France Region and ANSES (French Agency for Food, Environmental and Occupational Health & Safety) for the financial support of his PhD. Maria Kazour is financially supported by a PhD fellowship from the National Council for Scientific Research (Lebanon) and Université du Littoral Côte d’Opale (France).

Funding

This paper has been funded by the French National Research Agency (ANR) (ANR-15-CE34-0006-02), as part of the nanoplastics project and also by the French government and the Hauts-de-France Region in the framework of the project CPER 2014-2020 MARCO.

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Author notes

  1. Alexandre Dehaut and Guillaume Duflos contributed equally to this work.

Authors and Affiliations

  1. ANSES, Laboratoire de Sécurité des Aliments, Boulevard du Bassin Napoléon, 62200, Boulogne, France

    Ludovic Hermabessiere, Charlotte Himber, Béatrice Boricaud, Alexandre Dehaut & Guillaume Duflos

  2. UMR 8187, LOG, Laboratoire d’Océanologie et de Géosciences, CNRS, University of Littoral Côte d’Opale, University of Lille, 32 Avenue Foch, 62930, Wimereux, France

    Maria Kazour & Rachid Amara

  3. CNRS, National Centre for Marine Sciences, PO Box 534, Batroun, Lebanon

    Maria Kazour

  4. Laboratoire des Sciences de l’Environnement Marin (LEMAR), UMR6539/UBO/CNRS/IRD/IFREMER, Technopôle Brest-Iroise, Institut Universitaire Européen de la Mer, rue Dumont d’Urville, 29280, Plouzané, France

    Anne-Laure Cassone, Ika Paul-Pont & Philippe Soudant

  5. ANSES, Plateforme PAS, Laboratoire de Fougères, 10 B rue Claude Bourgelat, Javené, 35300, Fougères, France

    Michel Laurentie

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  1. Ludovic Hermabessiere
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Hermabessiere, L., Himber, C., Boricaud, B. et al. Optimization, performance, and application of a pyrolysis-GC/MS method for the identification of microplastics. Anal Bioanal Chem 410, 6663–6676 (2018). https://doi.org/10.1007/s00216-018-1279-0

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