High-performance liquid chromatographic determination of glyphosate in water and plant material after pre-column derivatisation with 9-fluorenylmethyl chloroformate

This paper describes a robust and sensitive HPLC method for determination of glyphosate in water and plant material after pre-column derivatisation with 9-fluorenyhmethyl chloroformate (FMOC-Cl) using single and coupled polymeric amino columns, respectively. New findings about optimisation of the derivatisation reaction and chromatographic behaviour of glyphosate and AMPA on polymeric amino column are also presented. The best HPLC conditions for the separation of glyphosate and AMPA in water samples were achieved using a single polymeric amino column and mobile phase at pH 10 which contained 55% (v/v) acetonitrile and 50mM phosphate buffer. The method was validated by analysing 10 fortified rainwater samples at a level of 1 mug/l. The average recovery was 94% with relative standard deviation (R.S.D.) of 5.4% and the method detection limit of 0.16 mug/l. The HPLC separation of glyphosate (only) in plant material entailed the coupling of two polymeric amino columns via a switching valve to separate interfering products from the desired analyte. The method was validated using grass samples spiked at the level of 1 mg/kg and gave a method detection limit of 0.3 mg/kg for glyphosate and a recovery of 82.4% with R.S.D. of 10.3%. (C) 2003 Elsevier B.V. All rights reserved.