Speciation of phenyltin(IV) compounds using high-performance liquid chromatography. Part 2: The direct analysis of mixed standard solutions of triphenyltin halides/pseudohalide and of triphenyltin carboxylates containing functional group variations in the esteryl moiety

Simultaneous speciation of mixed standard solutions of triphenyltin halides (triphenyltin chloride, bromide, iodide) and pseudohalide (triphenyltin isothiocyanate) has been achieved with reversed‐phase high‐performance liquid chromatography on a Waters Spherisorb S5W ODS‐2 (octadecyl‐silica) column. An isocratic mixture of 95:5 (v/v) acetonitrile:water was used as the mobile phase at a flow rate of 1 ml min−1. A series of selected triphenyltin carboxylates, Ph3SnOCOZ, where Z = Me, Ph, CH:CHPh, CH:NOMe, CH2SC5H4N and CH2SC(S)NMe2, was also similarly analysed using this system with two separate isocratic elutions using 100% acetonitrile and 96:4 (v/v) acetonitrile:water as the mobile phase. UV detection was done at 254 nm and the total run time for each analysis was less than 3 min. The detection limits for all the phenyltin(IV) compounds were in the range 0.01–0.03 ppm. Spiked water samples containing the triphenyltin carboxylates could also be simultaneously analysed by the above method without the need for any prior derivatization, following extraction with hexane. Pretreatment of the aqueous sample with NaCl/HCl and of the organic phase with hexamethylphosphoramide enabled recoveries of about 80% of the triphenyltins. Copyright © 2002 John Wiley & Sons, Ltd.