In this paper, we investigate the sample preparation and analysis process in order to achieve adequate results for surface water collected from rivers that flow through swamps and are consequently rich in organic matter. We show that matrix effects in glyphosate determination can be reduced by optimizing sample volume, liquid chromatography (LC) mobile phase buffer concentration and pH as well as gradient speed. Also, aspects of derivatization procedure (borate buffer concentration, fluorenylmethyloxycarbonyl chloride concentration) and their influence on accuracy are considered in detail. We encountered a cross-talk effect in the mass spectra, interfering with quantization during analysis, which was removed by optimizing MS parameters. As a result it was demonstrated that isotope-labelled internal standard with just one 13C atom is sufficient for the analysis.
All these aspects were found to strongly impact the accuracy of the glyphosate determination but have received little or no attention in earlier works. We propose a reliable solid phase extraction and LC/ESI/MS/MS method for determination of glyphosate in organic-rich waters and demonstrate that LoD can be decreased by about two times using an ESI nebulizer with a modified design.
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This work has been supported by the grant No. 8373 from the Estonian Science Foundation, by PUT 34 from the Estonian Research Council, by the Estonian National Research and Infrastructure development programme of measure 2.3 “Promotion of development activities and innovation” (Regulation No. 34) funded by the Estonian Enterprise foundation and by the institutional research grant IUT21-2 from the Estonian Ministry of Education and Science.
Responsible editor: Philippe Garrigues
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Toss, V., Leito, I., Yurchenko, S. et al. Determination of glyphosate in surface water with high organic matter content. Environ Sci Pollut Res 24, 7880–7888 (2017). https://doi.org/10.1007/s11356-017-8522-7
- Matrix effect
- Mass spectrometry
- Electrospray ionization