Determination of glyphosate and aminomethylphosphonic acid residues in Finnish soils by ultra‐high performance liquid chromatography–tandem mass spectrometry
Glyphosate [N-(phosphonomethyl) glycine] (GLY) adsorbs strongly in Finnish soils. A new method for GLY and its main degradation product, aminomethylphosphonic acid (AMPA) residues in clay soils (Protovertic Luvisol) was developed and validated. A new method was necessary because the previous one req...
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Elsevier
2023-12-01
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author | Sari Rämö Juho Välimäki Katri Siimes Jaana Uusi-Kämppä |
author_facet | Sari Rämö Juho Välimäki Katri Siimes Jaana Uusi-Kämppä |
author_sort | Sari Rämö |
collection | DOAJ |
description | Glyphosate [N-(phosphonomethyl) glycine] (GLY) adsorbs strongly in Finnish soils. A new method for GLY and its main degradation product, aminomethylphosphonic acid (AMPA) residues in clay soils (Protovertic Luvisol) was developed and validated. A new method was necessary because the previous one required laborious cleaning pre-treatments, and its recovery was quite poor (<40%–70%). In the new method, the earlier method's extraction solvent, 0.1 M potassium hydroxide (KOH), was replaced by more effective 0.6 M KOH. The old post-column high-performance liquid chromatography and fluorescence (HPLC-FLD) method was replaced by the ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) method. Compounds were identified as their fluorenyl methyl chloroformate (FMOC) derivatives by a multiple reaction monitoring (MRM) technique and quantified by an internal standard method utilising multipoint matrix-matched calibration. Glufosinate-ammonium (GLUF) was used to monitor the effectiveness of extraction with good recovery (80–119%). All calibration curves were found to be linear (R2 ≥ 0.98) in the studied calibration range (0.01–3.31 mg kg−1 in fresh soil). The repeatability and reproducibility were 25% and 28% for GLY, and 20% and 24% for AMPA in real research soil samples. The method was effective throughout the calibration range in all the studied Finnish agricultural soils. • An improved method was created to analyse glyphosate (GLY) and AMPA in Finnish clay soil. • The challenge caused by strong GLY adsorption on soil was solved by using multipoint matrix-matched calibration curve samples which were prepared identically with the research samples. • The method performed well in all tested clay, loam and sandy loam soils. |
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spelling | doaj.art-2d2931c1d3f544e18ddfbf726236d8a02023-12-04T05:22:34ZengElsevierMethodsX2215-01612023-12-0111102397Determination of glyphosate and aminomethylphosphonic acid residues in Finnish soils by ultra‐high performance liquid chromatography–tandem mass spectrometrySari Rämö0Juho Välimäki1Katri Siimes2Jaana Uusi-Kämppä3Natural Resources Institute Finland (Luke), Myllytie 1, Jokioinen 31600, Finland; Corresponding author.MTT Agrifood Research, Finland; current: KVVY Tutkimus Oy, Patamäenkatu 24, Tampere 33900, FinlandFinnish Environmental Institute (Syke), Latokartanonkaari 11, Helsinki 00790, FinlandNatural Resources Institute Finland (Luke), Tietotie 4, Jokioinen 31600, FinlandGlyphosate [N-(phosphonomethyl) glycine] (GLY) adsorbs strongly in Finnish soils. A new method for GLY and its main degradation product, aminomethylphosphonic acid (AMPA) residues in clay soils (Protovertic Luvisol) was developed and validated. A new method was necessary because the previous one required laborious cleaning pre-treatments, and its recovery was quite poor (<40%–70%). In the new method, the earlier method's extraction solvent, 0.1 M potassium hydroxide (KOH), was replaced by more effective 0.6 M KOH. The old post-column high-performance liquid chromatography and fluorescence (HPLC-FLD) method was replaced by the ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) method. Compounds were identified as their fluorenyl methyl chloroformate (FMOC) derivatives by a multiple reaction monitoring (MRM) technique and quantified by an internal standard method utilising multipoint matrix-matched calibration. Glufosinate-ammonium (GLUF) was used to monitor the effectiveness of extraction with good recovery (80–119%). All calibration curves were found to be linear (R2 ≥ 0.98) in the studied calibration range (0.01–3.31 mg kg−1 in fresh soil). The repeatability and reproducibility were 25% and 28% for GLY, and 20% and 24% for AMPA in real research soil samples. The method was effective throughout the calibration range in all the studied Finnish agricultural soils. • An improved method was created to analyse glyphosate (GLY) and AMPA in Finnish clay soil. • The challenge caused by strong GLY adsorption on soil was solved by using multipoint matrix-matched calibration curve samples which were prepared identically with the research samples. • The method performed well in all tested clay, loam and sandy loam soils.http://www.sciencedirect.com/science/article/pii/S221501612300393XDetermination of glyphosate and AMPA in Finnish soil by MRM-UHPLC-MS/MS-technique |
spellingShingle | Sari Rämö Juho Välimäki Katri Siimes Jaana Uusi-Kämppä Determination of glyphosate and aminomethylphosphonic acid residues in Finnish soils by ultra‐high performance liquid chromatography–tandem mass spectrometry MethodsX Determination of glyphosate and AMPA in Finnish soil by MRM-UHPLC-MS/MS-technique |
title | Determination of glyphosate and aminomethylphosphonic acid residues in Finnish soils by ultra‐high performance liquid chromatography–tandem mass spectrometry |
title_full | Determination of glyphosate and aminomethylphosphonic acid residues in Finnish soils by ultra‐high performance liquid chromatography–tandem mass spectrometry |
title_fullStr | Determination of glyphosate and aminomethylphosphonic acid residues in Finnish soils by ultra‐high performance liquid chromatography–tandem mass spectrometry |
title_full_unstemmed | Determination of glyphosate and aminomethylphosphonic acid residues in Finnish soils by ultra‐high performance liquid chromatography–tandem mass spectrometry |
title_short | Determination of glyphosate and aminomethylphosphonic acid residues in Finnish soils by ultra‐high performance liquid chromatography–tandem mass spectrometry |
title_sort | determination of glyphosate and aminomethylphosphonic acid residues in finnish soils by ultra high performance liquid chromatography tandem mass spectrometry |
topic | Determination of glyphosate and AMPA in Finnish soil by MRM-UHPLC-MS/MS-technique |
url | http://www.sciencedirect.com/science/article/pii/S221501612300393X |
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