Determination of Glyphosate and Its Metabolite AMPA (Aminomethylphosphonic Acid) in Cereals After Derivatization by Isotope Dilution and UPLC-MS/MS"

A straightforward analytical method has been developed for the determination of glyphosate and aminomethylphosphonic acid (AMPA), its major metabolite in cereals. This method entails a rapid extraction and derivatization with 9-fluorenylmethyl chloroformate followed by separation with a conventional reversed-phase rapid chromatography used in daily routine analysis and detection by electrospray ionization tandem mass spectrometry. To overcome matrix effects and compensate for any analyte losses during sample treatment, an isotopic dilution approach was used. Since 2010, the monitoring of cereals for the widely used herbicide glyphosate is obligatory to all European Union (EU)-member states, laid down in Commission Regulation (EC) No. 1213/2008. Hence, there is definitively a need for a reliable and easy-to-handle analytical method for monitoring of this compound. The proposed method can be run without having to make time-consuming changes on the equipment used for daily routine analysis. The analytical performance of the method was evaluated according to SANCO/10684/2009 criteria and demonstrated that this method is rugged and cost-effective, therefore suitable for monitoring purposes as well as legislative enforcements within the EU. The apparent recoveries of both analytes were between 97% and 113% with relative standard deviations less than 20%. The limits of quantification of glyphosate and AMPA were 0.02 mg/kg in cereal matrices. Finally, the accuracy of the method was assessed by analyzing a proficiency test material which was available from a previous round (EUPT-C4).