Dispersive liquid–liquid microextraction in combination with gas chromatographic–mass spectrometric determination is suggested for phenyltin compound analysis in aqueous solutions. The derivatization of the analytes with sodium tetraethylborate was carried out prior to the extraction. The effects of extraction and disperser solvent type, volume and extraction time on the extraction efficiency were investigated. Tetrachloromethane was used as an extraction solvent, ethanol was used as a disperser solvent, and hexachloroethane was used as an internal standard. The calibration graphs were linear from 46 ng l^–1 (monophenyltin), 161 ng l^–1 (diphenyltin) and 152 ng l^–1 (triphenyltin) up to 1 mg l^–1 (for all the analytes), correlation coefficients were 0.996–0.999, limits of detection were 14, 58 and 46 ng l^–1 for monophenyltin, diphenyltin and triphenyltin, respectively. Repeatabilities of the results were 4.6–17.3%. A possibility to apply the proposed method for phenyltin compound determination in river water was demonstrated.

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