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TitleDevelopment of a UHPLC-MS/MS method to enhance the detection of Glyphosate, AMPA and Glufosinate at sub-microgram / L levels in water samples
AbstractGlyphosate is the best-selling herbicide worldwide. The toxicity on ecosystems and the possible effects on human health have long been at the centre of a complex controversy concerning the authorisation for its use. The peculiar chemical-physical properties of glyphosate, AMPA and glufosinate make their determi- nation at trace levels in the water a real analytical challenge. All three compounds can be derivatised to less polar ones and FMOC-Cl (9-fluorenylmethyl chloroformate) is the most common pre-column derivati- sation reagent used for this analysis. It can be successfully combined with Ultra-High-Performance Liquid Chromatography with Mass Spectrometry (UHPLC-MS/MS) to determine all three analytes in one method as part of water monitoring programs. The developed method aims to determine glyphosate with AMPA and glufosinate at sub-micrograms/L levels in groundwater, surface and water by UHPLC-MS/MS after derivatisation with FMOC-Cl. The novelty of this method is its high simplicity, robustness and sensitivity allowing the identification and quantification of the compounds at the detection limits required by the European regulations (0.1 ?g /L). No pre-concentration or purification steps (by using Solid Phase Extrac- tion cartridges) are necessary for our method saving time and consumables costs. The method demon- strated an excellent linear relationship (R 2 >=0.999) in the concentration range from 0.025 to 10 ?g /L for glyphosate and AMPA and 0.025 to 5 ?g /L for glufosinate. The method Limit Of Quantification (LOQ) is 0.025 ?g/L, the lowest among all previously published studies, and it was demonstrated according to the European SANTE guidelines.
SourceJournal of chromatography A (Online)
KeywordsGlyphosate AMPA Glufosinate Pesticides UHPLC-MS/MS
JournalJournal of chromatography A (Online)
EditorElsevier Science, ,
Year2022
TypeArticolo in rivista
DOI10.1016/j.chroma.2022.463028
AuthorsClaudia Campanale, Mariangela Triozzi, Carmine Massarelli, Vito Felice Uricchio
Text466359 2022 10.1016/j.chroma.2022.463028 Glyphosate AMPA Glufosinate Pesticides UHPLC MS/MS Development of a UHPLC MS/MS method to enhance the detection of Glyphosate, AMPA and Glufosinate at sub microgram / L levels in water samples Claudia Campanale, Mariangela Triozzi, Carmine Massarelli, Vito Felice Uricchio CNR IRSA Glyphosate is the best selling herbicide worldwide. The toxicity on ecosystems and the possible effects on human health have long been at the centre of a complex controversy concerning the authorisation for its use. The peculiar chemical physical properties of glyphosate, AMPA and glufosinate make their determi nation at trace levels in the water a real analytical challenge. All three compounds can be derivatised to less polar ones and FMOC Cl 9 fluorenylmethyl chloroformate is the most common pre column derivati sation reagent used for this analysis. It can be successfully combined with Ultra High Performance Liquid Chromatography with Mass Spectrometry UHPLC MS/MS to determine all three analytes in one method as part of water monitoring programs. The developed method aims to determine glyphosate with AMPA and glufosinate at sub micrograms/L levels in groundwater, surface and water by UHPLC MS/MS after derivatisation with FMOC Cl. The novelty of this method is its high simplicity, robustness and sensitivity allowing the identification and quantification of the compounds at the detection limits required by the European regulations 0.1 g /L . No pre concentration or purification steps by using Solid Phase Extrac tion cartridges are necessary for our method saving time and consumables costs. The method demon strated an excellent linear relationship R 2 >=0.999 in the concentration range from 0.025 to 10 g /L for glyphosate and AMPA and 0.025 to 5 g /L for glufosinate. The method Limit Of Quantification LOQ is 0.025 g/L, the lowest among all previously published studies, and it was demonstrated according to the European SANTE guidelines. Published version https //doi.org/10.1016/j.chroma.2022.463028 Articolo in rivista Elsevier Science 1873 3778 Journal of chromatography A Online Journal of chromatography A Online Journal of chromatography A claudiacampanale CAMPANALE CLAUDIA TRIOZZI MARIANGELA vitofelice.uricchio URICCHIO VITO FELICE carmine.massarelli MASSARELLI CARMINE