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A sediment extraction and cleanup method for wide-scope multitarget screening by liquid chromatography–high-resolution mass spectrometry

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Abstract

Previous studies on organic sediment contaminants focused mainly on a limited number of highly hydrophobic micropollutants accessible to gas chromatography using nonpolar, aprotic extraction solvents. The development of liquid chromatography–high-resolution mass spectrometry (LC–HRMS) permits the spectrum of analysis to be expanded to a wider range of more polar and ionic compounds present in sediments and allows target, suspect, and nontarget screening to be conducted with high sensitivity and selectivity. In this study, we propose a comprehensive multitarget extraction and sample preparation method for characterization of sediment pollution covering a broad range of physicochemical properties that is suitable for LC–HRMS screening analysis. We optimized pressurized liquid extraction, cleanup, and sample dilution for a target list of 310 compounds. Finally, the method was tested on sediment samples from a small river and its tributaries. The results show that the combination of 100 °C for ethyl acetate–acetone (50:50, neutral extract) followed by 80 °C for acetone–formic acid (100:1, acidic extract) and methanol–10 mM sodium tetraborate in water (90:10, basic extract) offered the best extraction recoveries for 287 of 310 compounds. At a spiking level of 1 μg mL-1, we obtained satisfactory cleanup recoveries for the neutral extract—(93 ± 23)%—and for the combined acidic/basic extracts—(42 ± 16)%—after solvent exchange. Among the 69 compounds detected in environmental samples, we successfully quantified several pharmaceuticals and polar pesticides.

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Acknowledgements

We thank Jörg Ahlheim and Pedro Inostroza for sample collection. We also thank Melis Muz for reviewing the draft versions. We acknowledge funding by the SOLUTIONS Project supported by the European Union Seventh Framework Programme (FP7-ENV-2013-two-stage collaborative project) under grant agreement no. 603437. Chemaxon (Budapest, Hungary) is gratefully acknowledged for free academic licenses for Marvin and JChem for Excel.

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  1. Jens Prothmann

    Present address: Centre for Analysis and Synthesis, Department of Chemistry, Lund University, Getingev 60/Sölvegatan 39, Lund, Sweden

Authors and Affiliations

  1. Department of Effect-Directed Analysis, Helmholtz Centre for Environmental Research—UFZ, Permoserstr. 15, 04318, Leipzig, Germany

    Riccardo Massei, Harry Byers, Liza-Marie Beckers, Jens Prothmann, Werner Brack, Tobias Schulze & Martin Krauss

  2. Department of Ecosystem Analyses, Institute for Environmental Research, RWTH Aachen University, Worringerweg 1, Aachen, Germany

    Riccardo Massei, Harry Byers, Liza-Marie Beckers & Werner Brack

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  1. Riccardo Massei
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Correspondence to Riccardo Massei.

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The study was partly founded by the SOLUTIONS project supported by the European Union’s Seventh Framework Programme (FP7-ENV-2013-two-stage Collaborative project) under grant agreement no. 603437. The authors declare that they have no conflict of interest. This study does not contain any studies with human participants or animals performed by any of the authors. Additional informed consent was obtained from all individual participants for whom identifying information is included in this study.

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Massei, R., Byers, H., Beckers, LM. et al. A sediment extraction and cleanup method for wide-scope multitarget screening by liquid chromatography–high-resolution mass spectrometry. Anal Bioanal Chem 410, 177–188 (2018). https://doi.org/10.1007/s00216-017-0708-9

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  • DOI: https://doi.org/10.1007/s00216-017-0708-9

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