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Monitoring of triphenyltin (TPhT) in the environment, particularly to control its misuse in agriculture, is of great importance because of its high toxicity. In this work, methods for determination of TPhT residues in surface water and soil samples by liquid chromatography with tandem mass spectrometry (LC-MS/MS) were developed and validated. Different sample volumes and pH and elution solvent types and volumes were evaluated for solid phase extraction (SPE) of TPhT in surface water samples. The optimized conditions were 500 mg sorbent S