Determination of organohalogenated compounds in organic fertilizer using extraction with the aid of ultrasound and gas chromatography with electron capture detection

Wickert, Cristine; Adaime, Martha B.; Zanella, Renato

Palavras-chave: organohalogenated compounds, organic fertilizer, GC-ECD.

Resumo: The use of waste from livestock, such as poultry litter, is often employed in the agriculture as organic fertilizer. However, they may contain residues of wood preservatives, like organohalogenated compounds, from the shavings and sawdust used. In the present work a method for the determination of pentachlorophenol, 2,4,6-trichlorophenol, 2,4,6-trichloroanisol, 2,4,6-tribromophenol and 2,4,6-tribromoanisol residues in organic fertilizer using gas chromatography with electron capture detection (GC-ECD) was developed and validated. Several extraction procedures, using ultrasonic bath and probe, as well the association of mechanical agitation with ultrasonic bath in different conditions were evaluated and optimized. Better results were obtained using mechanical agitation associated to the ultrasonic bath, ethanol/acetic acid 9:1 (v/v) as solvent for extraction and florisil® for the extract clean-up before derivatization with anhydride acetic. The validated method presented detection limit from 11.3 to 22.5 μg kg-1 and good linearity. Accuracy, in terms of recovery, ranged from 81.3 to 110.8%, with adequate precision (RSD <12.4%). Results from the validation and application steps allow to conclude that the proposed method is appropriate for the determination of organohalogenated compounds in organic fertilizer in routine analyses.

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