Abstract
A selective procedure is developed for the determination of glyphosate, aminomethylphosphonic acid, and glufosinate in raw materials of plant origin by chromatography–mass spectrometry. The limit of quantification for glyphosate is 0.1 mg/kg and for glufosinate and aminomethylphosphonic acid, 0.4 mg/kg. The procedure is based on the extraction of analytes from a sample with deionized water acidified with hydrochloric acid, solid-phase purification followed by derivatization with 9-fluorenylmethoxycarbonyl chloride, and the additional purification of the derivatives on a sorbent with weak cation-exchange properties. The extraction and purification procedures for the extracts are optimized. The effect of matrix components on the chromatographic separation and detection of glyphosate on chromatographs–mass spectrometers of various types is studied. Validation of the developed procedure showed that the relative expanded uncertainty lies in the range from 15 to 25%.
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