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The accumulation of organophosphorus type herbicides has been observed worldwide in the environment (i.e. soil, water), together with their appearance in foods of plant origin. This paper reports a new liquid chromatography–isotope dilution–tandem mass spectrometric method (LC-IDMS) for the analysis of glufosinate (GLUF), glyphosate (GLY) and its main metabolite, aminomethylphosphonic acid (AMPA), in challenging food samples. Sample preparation is based on aqueous extraction with ethylenediaminetetraacetic acid solution, followed by solid-phase extraction (SPE) on mixed-mode cation exchange cartridges to remove matrix constituents before derivatization with 9-fluorenylmethoxycarbonyl chloride (FMOC-Cl). Derivatized samples were cleaned up on hydrophilic modified polymeric SPE cartridge. This two-step SPE supported sample preparation approach, and the LC-IDMS separation carried out in negative ionization mode resulted in fit-for-purpose recovery (81–118%) and precision (4–18%) in the validation of glutamate loaded spice mix, mushroom, maize and cherry samples. Amino acid content influencing FMOC derivatization efficiency was estimated with a HILIC-MS/MS setup. Multiple reaction monitoring (MRM) was assisted with high-resolution (QTOF) accurate mass data on the FMOC-derivatized GLUF, GLY and AMPA standards. The limit of quantification (LOQ) was 0.005 mg/kg for all the three analytes. The method was successfully applied on quality control samples (oat and arugula) with fit-for-purpose accuracy (99–120%) and on other nineteen real samples, where GLY and AMPA were detected in the range between 0.005 and 0.069 mg/kg.

Determination of Aminophosphonate Herbicides in Glutamate Loaded Spice Mix by LC-IDMS and Method Extension to Other Food Matrices