In this work, the capability of a hybrid tandem technique of LCMS-IT-TOF was examined for speciation of tripropyltin (TPrT), tributyltin (TBT), tripentyltin (TPeT) and triphenyltin (TPhT) and a relatively fast and accurate method was developed for their determination in aqueous solutions. In this context, several chromatographic parameters were studied such as chromatographic column, mobile phase, flow rate and gradient program in order to optimise the separation of the above species. Optimum separation was achieved using reverse phase C18 bonded-silica column. The mobile phase consisted of water and methanol and acetic acid at a total flow rate of 0.4 mL min–1 and the separation was completed in less than 8 min. Determination of the analytes was performed based on the signal of characteristic ions for each particular triorgano-tin compound. The detection limits of the set of the above four triorgano-tin species were ranged between 13 – 45 pg as absolute mass of Sn injected into the column and the relative standard deviation was ranged between 4.3 – 9.9 %. Finally, the performance characteristics of the method were compared to those reported in literature using similar tandem LC-MS techniques.