1988 Volume 29 Issue 2 Pages 141-145_1
A gas chromatographic method was developed for the determination of a trace amount of tributyltin compounds in fish samples by the use of a Sep-pak® Florisil cartridge for clean-up.
Tributyltin compounds in a flesh sample of fish were extracted as tributyltin chloride (TBTC) by homogenizing the sample with a hydrochloric acid-methanol mixture, and TBTC was transferred to the hexane phase by liquid-liquid extraction. The extract was charged onto a Sep-pak® Florisil cartridge. After washing of the cartridge successively with hexane-ethanol (1:1) mixture and hexane, TBTC was eluted with hexane-acetic acid (50:1) mixture. The eluate was washed with 1M hydrochloric acid and concentrated in a rotary evaporator. The concentrate was subjected to gas chromatographic separation on a 10% KOCL-Sn column with electron capture detection.
The calibration curve was linear in the range of 0.02-0.4μg/ml. The detection limit of TBTC in fish samples was 0.003μg/g. The recovery of TBTC from fish spiked at 0.04μg/g level was more than 88%. The analytical results were also presented for various fish samples collected at the Sea of Japan and fish farms.
