Simultaneous Determination of Ethidimuron, Methabenzthiazuron, and Their Two Major Degradation Products in Soil

Lagarde, F.; Führ, F.; Dressel, J.; Pütz, T.

doi:10.1021/jf061042v

Journal Article

PreJuSER-52843

Simultaneous Determination of Ethidimuron, Methabenzthiazuron, and Their Two Major Degradation Products in Soil

Lagarde, F. ; Pütz, T.FZJ* ; Dressel, J. ; Führ, F.FZJ*

2006
American Chemical Society (ACS) Washington, DC [u.a.]

Journal of agricultural and food chemistry 54, 7450 - 7459 (2006) [10.1021/jf061042v]

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Please use a persistent id in citations: http://hdl.handle.net/2128/798 doi:10.1021/jf061042v

Abstract: An analytical method has been developed for the quantification of two herbicides (ethidimuron and methabenzthiazuron) 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 at 282 nm. FBE conditions were established to provide efficient extraction without degradation of the four analytes. (14)C-labeled compounds were used for the optimization of extraction and purification steps and for the determination of related efficiencies. Extraction was optimal using a fexIKA extractor operating at 110 degrees C for three cycles (total time = 95 min) with 75 g of soil and 150 mL of a 60:40 v/v acetone/water mixture. Extracts were further purified on a 500 mg silica SPE cartridge. Separation was performed on a C18 Purosphere column (250 mm x 4 mm i.d.), at 0.8 mL min(-1) and 30 degrees C with an elution gradient made up of phosphoric acid aqueous solution (pH 2.2) and acetonitrile. Calibration curves were found to be linear in the 0.5-50 mg L(-1) concentration range. Besides freshly spiked soil samples, 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 3 microg kg(-1) of dry soil and limits of quantification between 8 and 10 microg kg(-1) of dry soil. An attempt to improve these performances by using fluorescence detection following postcolumn derivatization by orthophthalaldehyde-mercaptoethanol reagent was unsuccessful.

Keyword(s): Benzothiazoles: analysis (MeSH) ; Benzothiazoles: chemistry (MeSH) ; Chromatography, High Pressure Liquid: methods (MeSH) ; Herbicides: analysis (MeSH) ; Methylurea Compounds: analysis (MeSH) ; Methylurea Compounds: chemistry (MeSH) ; Photolysis (MeSH) ; Sensitivity and Specificity (MeSH) ; Soil: analysis (MeSH) ; Solutions (MeSH) ; Benzothiazoles ; Herbicides ; Methylurea Compounds ; Soil ; Solutions ; ethidimuron ; methabenzthiazuron ; J ; ethidimuron (auto) ; methabenzthiazuron (auto) ; metabolites (auto) ; soils (auto) ; fexIKA extraction (auto) ; SPE purification (auto) ; HPLC-DAD (auto) ; fluorescence (auto)