A synthetic approach to ten metabolites of iodosulfuron-methyl sodium and metsulfuron-methyl was performed and reported in this study. The compounds of interest were prepared by controlled hydrolytic degradation of active substances or by de novo synthesis from commercially available triazine precursor 10. Obtained compounds were characterized by IR, NMR, and elemental analysis techniques. Metabolites and active substances were utilized during the development of a separation and quantification method using reversed-phase high-performance liquid chromatography coupled with tandem mass spectrometry. The validated method was applied for the analysis of all studied compounds in the extracts from water samples collected from the Vistula river (Toruń, Poland).
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