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

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