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| - Simultaneous Determination of Ethidimuron,Methabenzthiazuron, and Their Two Major DegradationProducts in Soil
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| - An analytical method has been developed for the quantification of two herbicides (ethidimuron andmethabenzthiazuron) and their two main soil derivatives. This method involves fluidized-bed extraction(FBE) prior to cleanup and analysis by reverse-phase liquid chromatography with UV detection at282 nm. FBE conditions were established to provide efficient extraction without degradation of thefour analytes. 14C-labeled compounds were used for the optimization of extraction and purificationsteps and for the determination of related efficiencies. Extraction was optimal using a fexIKA extractoroperating at 110 °C for three cycles (total time = 95 min) with 75 g of soil and 150 mL of a 60:40 v/vacetone/water mixture. Extracts were further purified on a 500 mg silica SPE cartridge. Separationwas performed on a C18 Purosphere column (250 mm × 4 mm i.d.), at 0.8 mL min-1 and 30 °C withan elution gradient made up of phosphoric acid aqueous solution (pH 2.2) and acetonitrile. Calibrationcurves were found to be linear in the 0.5−50 mg L-1 concentration range. Besides freshly spiked soilsamples, method validation included the analysis of samples with aged residues. Recovery values,determined from spiked samples, were close to 100%. Limits of detection ranged between 2 and 3μg kg-1 of dry soil and limits of quantification between 8 and 10 μg kg-1 of dry soil. An attempt toimprove these performances by using fluorescence detection following postcolumn derivatization byorthophthalaldehyde−mercaptoethanol reagent was unsuccessful. Keywords: Ethidimuron; methabenzthiazuron; metabolites; soils; fexIKA extraction; SPE purification;HPLC-DAD; fluorescence
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