Bestimmung von Atrazin,Terbutylazin und ihrer Desethyl- sowie Hydroxymetaboliten in Boden mittels SFE und HPLC/UV-DAD |
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| Authors: | M Kolb B Englert |
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| Abstract: | Determination of Atrazine, Terbutylazine and their Deethyl- and Hydroxymetabolites in Soil by SFE and HPLC/UV-DAD The supercritical fluid extraction (SFE) (CO2 and CH3OH as modifier) of the herbicides atrazine and terbutylazine as well as their deethyl- and hydroxymetabolites from soil was investigated. The analytes were determined after extraction by HPLC/UV-DAD using a C18 column. The limits of detection of the chromatographic step were between 0.01 μg/mL and 0.07 μg/mL, the relative standard deviations between 0.8% and 1.4%. With the aid of a control chart, the stability of the chromatographic system was evaluated. For extraction, soil was spiked with 5 μg/g for each component. For SFE, CO2 and methanol as modifier were used, and a pressure program was applied. Beside SFE, Soxhlet extraction with methanol and a solid-liquid extraction with acetone/water by shaking were carried out. For chlorine-containing triazines, the recovery rates were comparable for all extraction methods. The following recovery rates for SFE were obtained: deethylterbutylazine 77.4%, terbutylazine 80.2%, deethylatrazine 87.4%, atrazine 92.6%. However, the recovery rates for the hydroxymetabolites (4.1% for hydroxyatrazine, 21% for hydroxyterbutylazine) were not satisfying compared with the “classical” methods of extraction (above 50%). The limits of detection for the total process (SFE and HPLC/UV-DAD) estimated by the signal to noise ratio amounted 0.08 μg/g soil for chlorine-containing derivates, for hydroxyatrazine 2…3 μg/g, and for hydroxyterbutylazine 0.8 μ/g. |
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| Keywords: | Triazine Herbicides Supercritical Fluid Extraction SFE Metabolites Soil |
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