Determination of tributyltin and triphenyltin compounds in hair and fish using a hydrolysis technique and gas chromatography with flame photometric detection.

A hydrolysis technique and a GC method are described for the determination of tributyltin and triphenyltin compounds in human hair and fish tissue. A sample was hydrolysed with a potassium hydroxide-ethanol-water solution. Tributyltin and triphenyltin compounds in the hydrolysate were extracted with toluene, and then impurities in the extract were eliminated with anion- and cation-exchange resins. After propylation of the organotin compounds, a yellow impurity was removed with a Sep-Pak florisil cartridge, and the two propylated organotin compounds were separated using a silicone OV-1 GC column and determined by flame photometric detection. The limits of determination of tributyltin and triphenyltin compounds in the sample were 5 and 10 ng g-1, respectively, in their chloride forms. The recoveries of tributyltin chloride from hair samples were 78.8 and 90.8%, respectively, when the spiked amounts were 20 and 200 ng. The recoveries of triphenyltin chloride from hair samples were 71.7 and 72.7%, respectively, when the spiked amounts were 40 and 400 ng. The recoveries of the organotin compounds from fish were similar to the recoveries from hair.