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Determination of trihalomethanes in soil matrices by simplified quick, easy, cheap, effective, rugged and safe extraction and fast gas chromatography with electron capture detection

Herrero Martín, Sara, García Pinto, Carmelo, Pérez Pavón, José Luis, Moreno Cordero, Bernardo
Journal of chromatography 2010 v.1217 no.30 pp. 4883-4889
centrifugation, chloroform, detection limit, ethyl acetate, gardens, gas chromatography, magnesium sulfate, soil, soil sampling
A method based on QuEChERS extraction is proposed for the determination of trihalomethanes (chloroform, bromodichloromethane, dibromocloromethane and bromoform) in soil samples. The new version of QuEChERS adapted to soil samples consists of liquid extraction with ethyl acetate, the addition of water to moisten the samples, salting-out partitioning of the water with anhydrous MgSO₄, and direct injection of the organic extract, obtained after the centrifugation step, into the gas chromatograph. This simplified extraction procedure maintains the advantages of the original method and avoids some steps, making the final procedure simpler, faster, and cheaper, with the consequent reduction in errors associated with sample manipulation. The experimental conditions of the analytical method, based on fast gas chromatography (FGC) and micro-electron capture detection (μECD), were optimized. The column and oven program used allowed fast separation of the compounds in less than 4min and the total analysis cycle time was as short as 10min. The existence of a matrix effect was checked and the analytical conditions of the method were studied in a fortified garden soil sample. The highly sensitive and selective detector used afforded to detection limits in the order of ng/kg for the target compounds. To validate the proposed method two certified reference materials (CRMs) were analyzed.