[en] A new sensitive and selective analytical methodology to quantify glyphosate (GLY), aminomethylphosphonic acid (AMPA), and glufosinate (GLU) in both soil and earthworms (Allolobophora chlorotica) was developed. The extraction and purification methods were optimized. The samples were extracted with various aqueous solutions (HNO3, H2O, KOH and borate buffer) and derivatized with 9-Fluorenylmethyl chloroformate (FMOCCl). To optimize the extraction step, a method to remove the excess FMOCCl was applied based on liquid-liquid extraction with diethyl ether. The purification of derivatized extracts was carried out using XLB solid phase extraction (SPE) cartridges before internal standard quantification by liquid chromatography coupled to tandem mass spectrometry (LC/MS/MS). The elution step was optimized to obtain the best recoveries possible, which was with acidic methanol (1% formic acid) (67% for GLY, 70% for GLU and 65% for AMPA). The extraction and purification method followed by analysis of the two herbicides and AMPA in soils using LC/MS/MS determined limit of quantification (LOQ) values of 0.030 μg g - 1 for GLY, 0.025 μg g - 1 for AMPA and 0.020 µg g - 1 for GLU . For earthworms, LOQ were 0.23 μg g - 1 for GLY, 0.20 μg g - 1 for AMPA and 0.12 μg g - 1 for GLU. . The developed method was applied to determine these compounds in natural soils and earthworms.
Disciplines :
Chemistry
Author, co-author :
Delhomme, Olivier; Université de Strasbourg, CNRS-UMR 7515, ICPEES, 67087, Strasbourg, France, Université de Lorraine, 57070, Metz, France
Rodrigues, Anaïs ; Université de Liège - ULiège > Molecular Systems (MolSys) ; Université de Strasbourg, CNRS-UMR 7515, ICPEES, 67087, Strasbourg, France
Hernandez, Ana; Université de Strasbourg, CNRS-UMR 7515, ICPEES, 67087, Strasbourg, France
Chimjarn, Supansa; Université de Strasbourg, CNRS-UMR 7515, ICPEES, 67087, Strasbourg, France
Bertrand, Colette ; Université Paris-Saclay, INRAE, AgroParisTech, UMR ECOSYS, 78026, Versailles, France
Bourdat-Deschamps, Marjolaine; Université Paris-Saclay, INRAE, AgroParisTech, UMR ECOSYS, 78850, Thiverval-Grignon, France
Fritsch, Clémentine; Laboratoire Chrono-environnement, UMR 6249 CNRS - Université de Franche-Comté Usc INRAE, 16 route de Gray 25030 Besançon cedex, France
Pelosi, Céline; INRAE, Avignon Université, UMR EMMAH, 84000, Avignon, France
Nélieu, Sylvie; Université Paris-Saclay, INRAE, AgroParisTech, UMR ECOSYS, 78850, Thiverval-Grignon, France
Millet, Maurice; Université de Strasbourg, CNRS-UMR 7515, ICPEES, 67087, Strasbourg, France
Language :
English
Title :
A method to assess glyphosate, glufosinate and aminomethylphosphonic acid in soil and earthworms.
INRAE - Institut National de Recherche pour l'Agriculture, l'Alimentation et l'Environnement
Funding text :
This study was carried out within the framework of the “PING” research project, funded by the Métaprogramme INRAE SMaCH Call 2017. The study also benefited from the samples collected during the “RESCAPE” research project, led by the Ministry for Agriculture and Food and the Ministry for an Ecological and Solidary Transition, with the financial support of the French Biodiversity Agency on “Resistance and Pesticides”, with the fees for diffuse pollution coming from the Ecophyto Plan through the national agency ONEMA. We thank the ZAPVS for help accessing the field plots.
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