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Quantitative analysis of glyphosate, glufosinate and AMPA in irrigation water by in situ derivatization - dispersive liquid-liquid microextraction combined with UPLC-MS/MS

Abstract

A novel method was developed for the sensitive, cheap and fast quantitation of glyphosate, glufosinate and aminomethylphosphonic acid (AMPA) in irrigation water by in-situ derivatization and dispersive liquid-liquid extraction (DLLME) combined with ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Water samples were filtered with a 0.22 μm nylon filter, pH adjusted to 9 with ammonium bicarbonate and derivatized with fluorenylmethyloxycarbonyl chloride (FMOC-Cl). Afterwards, DLLME was applied to concentrate the compounds of interest, which were then analyzed by UPLC-MS/MS. The best results were obtained when acetone and dichloromethane were used as dispersive and extraction solvents, respectively. Two-level full factorial designs and a central composite design were applied to select the most appropriate derivatization and DLLME conditions. The method performance was evaluated according to the SANTE/11945/2015 guidelines and was linear in the 1.0 to 200 µg/L range for glyphosate, glufosinate and AMPA, with r2 ≥ 0.997 and individual residuals <13%. Repeatability (RSDr) and within-laboratory reproducibility (RSDwr) ranged from 2.7 to 9.1% and from 3.4 to 14.3%, respectively, and the trueness between 94.9 and 118.1%. The limits of detection were of 0.35, 0.05 and 0.10 µg/L for glyphosate, glufosinate and AMPA, respectively and the limits of quantitation were of 1.0 µg/L for all three compounds. The developed method was successfully applied to the analysis of irrigation water (surface and groundwater). No sign of the three compounds was detect in the groundwater samples but glyphosate was quantified in surface waters.

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Publication details

The article was received on 24 Nov 2017, accepted on 02 Jan 2018 and first published on 03 Jan 2018


Article type: Paper
DOI: 10.1039/C7AY02722B
Citation: Anal. Methods, 2018, Accepted Manuscript
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    Quantitative analysis of glyphosate, glufosinate and AMPA in irrigation water by in situ derivatization - dispersive liquid-liquid microextraction combined with UPLC-MS/MS

    E. Pinto, A. G. Soares and I. M. P. L. V. Ferreira, Anal. Methods, 2018, Accepted Manuscript , DOI: 10.1039/C7AY02722B

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