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Optimization of extraction procedure and chromatographic separation of glyphosate, glufosinate and aminomethylphosphonic acid in soil

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Abstract

Analysing herbicides in soil is a complex issue that needs validation and optimization of existing methods. An extraction and analysis method was developed to assess concentrations of glyphosate, glufosinate and aminomethylphophonic acid (AMPA) in field soil samples. After testing extractions by accelerated solvent extraction and ultrasonic extraction, agitation was selected with the best recoveries. Water was preferred as solvent extraction because it resulted in a cleaner chromatogram with fewer impurities than was the case with alkaline solvents. Analysis was performed by FMOC pre-column derivatization followed by high-performance liquid chromatography (HPLC) on a 300 mm C18 column which permitted enhanced separation and sensitivity than a 250 mm C18 column and increased resistance than the NH2 column for soil samples. This extraction and analysis method allowing a minimum of steps before the injection in the HPLC with fluorescence detection is efficient and sensitive for a clay-loamy soil with detection limits of 103 μg kg−1 for glyphosate, 15 μg kg−1 for glufosinate and 16 μg kg−1 for AMPA in soil samples.

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Acknowledgements

This work was financially supported by grants from the Agence De l’Environnement et de la Maîtrise de l’Energie (ADEME), the Conseil Régional de Franche-Comté, the RE.A.LI.SE network, the Alsace région and the network of CNRS, Evaluer et Réduire l’Impact de la Chimie sur l’Environnement (ERICHE). We thank all trainees of the lab LMSPC, which took part in the realisation of this work by their technical assistance. We thank also Brice Mourier for his help for the soil characterisation.

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  1. Olivier Delhomme

    Present address: Laboratoire de Spectrométrie de Masse et de Chimie Laser, Université Paul Verlaine de Metz, 1 Boulevard Arago, 57 078, Metz Cedex 03, France

Authors and Affiliations

  1. Department of Chrono-Environment, University of Franche-Comté, UMR UFC/CNRS 6249 usc INRA, Place Leclerc, 25030, Besançon Cedex, France

    Coline Druart & Annette de Vaufleury

  2. Equipe de Physico-Chimie de l’Atmosphère-LMSPC (UMR 7515 CNRS-Université de Strasbourg), 1 rue Blessig, 67084, Strasbourg Cedex, France

    Olivier Delhomme, Evodie Ntcho & Maurice Millet

Authors
  1. Coline Druart
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  2. Olivier Delhomme
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  3. Annette de Vaufleury
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  4. Evodie Ntcho
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  5. Maurice Millet
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Correspondence to Maurice Millet.

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Druart, C., Delhomme, O., de Vaufleury, A. et al. Optimization of extraction procedure and chromatographic separation of glyphosate, glufosinate and aminomethylphosphonic acid in soil. Anal Bioanal Chem 399, 1725–1732 (2011). https://doi.org/10.1007/s00216-010-4468-z

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  • DOI: https://doi.org/10.1007/s00216-010-4468-z

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