This paper describes a low-cost reversed-phase sequential injection chromatography method for the determination of glyphosate and aminomethylphosphonic acid in environmental samples. The method is based on the pre-column conversion of glyphosate to glycine by hypochlorite, followed by reaction with o-phthaldialdehyde in presence of 2-mercaptoethanol in borate buffer (pH 9.5) to produce the fluorescent 1-(2′-hydroxyethylthio)-2-N-alkylisoindole. In addition to producing detectable fluorescent indoles, the pre-column derivatization also decreases the polarity of the analytes, favoring their retention on a C18 monolithic column. The isocratic reversed-phase chromatography enabled the separation of both glyphosate and aminomethylphosphonic acid derivatives from polar compounds such as organic acids, humic substances, and carbohydrates which are commonly found in waters and soil extracts. This separation minimizes the laborious sample preparation procedures prior to the analysis. The linear response was observed for concentrations between 0.10 and 12.8 μM. The limits of detection and quantification were 0.03 and 0.10 μM (glyphosate), and 0.015 and 0.050 μM (aminomethylphosphonic acid). At the 0.10 μM concentration level, the relative standard deviations were 21 and 25% for aminomethylphosphonic acid and glyphosate, respectively (n = 5). Recoveries between 80 and 120% were found in the determination of glyphosate and aminomethylphosphonic acid in spiked lake waters (0.80 to 6.4 μM). The method was applied in the determination of kinetic and thermodynamic parameters related to the adsorption of glyphosate on two horizons of an Alfisol from the Paraná State in South Brazil.
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This work was funded by grants 2013/18507-4 from the São Paulo Research Foundation (FAPESP) and 303940/2017-4 from the National Council for Scientific and Technological Development (CNPq). EAOP received MSc fellowship from CNPq (Grant 134790/2016-2).
Compliance with ethical standards
Conflict of interest
The authors declare that they have no conflict of interest.
This article does not contain any studies made with humans or animals.
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