Improved coupled-column liquid chromatographic method for the determination of glyphosate and aminomethylphosphonic acid residues in environmental waters

An existing method for the determination of glyphosate and its main metabolite aminomethylphosphonic acid (AMPA) in water has been improved. It is based on precolumn derivatization with the fluorescent reagent 9-fluorenylmethylcloroformate (FMOC) followed by large-volume injection in a coupled-column LC system using fluorescence detection (LC–LC–FD). The derivatization step was slightly modified by changing parameters such as volume and/or concentration of sample and reagents to decrease the limits of quantification (LOQ) of glyphosate and AMPA to 0.1 μg/l. Additionally, the use of Amberlite® IRA-900 for preconcentration of glyphosate, prior to the derivatization step, was investigated; the LOQ of glyphosate was lowered to 0.02 μg/l. Drinking, surface and ground water spiked with glyphosate and AMPA at 0.1–10 μg/l concentrations were analysed by the improved LC–LC–FD method. Recoveries were 87–106% with relative standard deviations lower than 8%. Drinking and ground water spiked with glyphosate at 0.02 and 0.1 μg/l were analysed after preconcentration on the anion-exchange resin with satisfactory recoveries (94–105%) and precision (better than 8%).