A simple, high-throughput method for quantification of glyphosate [N-(phosphomethyl)glycine] and AMPA (aminomethylphosphoric acid) was initially developed and validated in about 40 raw agricultural commodities (RAC) and processed commodities (juices, flours, whole grains, legumes, tubers, nuts/seeds, etc.). Stable isotope labeled internal standards and a derivatization procedure with FMOC (fluorenylmethyloxycarbonyl chloride) were employed for the analysis by liquid chromatography-tandem mass spectrometry. The primary goals of the method were to provide a single analytical workflow for use on all matrices, with a target limit of quantitation (LOQ) of 0.01 – 0.05 mg/kg for both glyphosate and AMPA.  Employing the method for routine analysis demonstrated excellent performance on raw and minimally processed agricultural commodities and also highlighted the need for modifications and further development for applicability to more complex matrices, such as botanical extracts. Inclusion of these matrices necessitated further development work and reassessment of previous techniques utilized for sample cleanup.  Validation of the method modifications provided additional capabilities for the analytical method and satisfied the goal of expanding the method scope to more complex sample matrices.

Trials and tribulations of glyphosate analysis in raw agricultural commodities, foods, and dietary supplements

2019 Fall National Meeting

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