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 Strata C18-E, 100 mL of the sample, pH adjusted to 9.0 and 1 mL of methanol containing acetic acid as the eluent. For a 10 g soil sample, the extraction was established using a modified QuEChERS method with 10 mL of acidified acetonitrile followed by a clean-up step by dispersive solid phase extraction (dSPE) with C18. A full factorial 2³ design of experiments was applied to optimize the sample preparation method for soil samples. Practical method limits of quantification were 0.1 μg L⁻¹ and 10 μg kg⁻¹ for surface water and soil samples, respectively. Satisfactory accuracy, with recoveries from 86 to 107% for surface water and 72 to 87% for soil samples, as well as good precision, with an overall relative standard deviation (RSD) from 3 to 8% was observed. The validated methods were applied to real samples and some residues of TPhT were found, especially in soil samples (30 to 190 mg kg⁻¹), indicating the suitability for routine analysis.