Determination of tributyltin compounds in fish and shell-fish by GC using electron capture detector.

TAKEUCHI Masahiro, MIZUISHI Kazuko, YAMANOBE Hideo, WATANABE Yohya

doi:10.2116/bunsekikagaku.36.3_138

To obtain reproducible peaks of tributyltin chloride (TBTC) in GC using an electron capture detector (ECD), the pretreatment of GC column with 0.1 M hydrochloric acid (HCl)-acetone solution and the simultaneous injection of 0.01 M HCl-acetone solution with sample solutions have been investigated, and the results were applied to the determination of tributyltin compounds in fish and shell-fish samples : Tributyltin compounds in the samples were determined by ECD-GC after converting to TBTC. Five grams of homogenized fish arid shell-fish was extracted twice with 70 ml of hexane-ethyl ether (3 : 1, v/v) mixture in the presence of HCl. The combined extract was poured into a Florisil column (3 g of Florisil and 2 g of anhydrous sodium sulfate), then 50 ml of acetone and 40 ml of hexane-ethyl ether-acetic acid (75 : 25 : 1, v/v/v) mixture were eluted. The latter eluate was collected in a pear-shaped flask, concentrated by a rotary evaporator, and 3 μl portion of the concentrate was injected, together with 2 μl of 0.01 M HCl-acetone solution, into a gas chromatograph equipped with {10% Thermon-HG on Chromosorb W (AW-DMCS), 2.5 m×3.2 mm i.d.} column pretreated with 100150 μl of 0.1 M HCl-acetone solution. The total content of tributyltin comopounds could be caluculated from the peak height of TBTC in the chromatogram. The recovery and the relative standard deviation of this method at 2.0 μg level of bis(tributyltin) oxide added (2.16 μg as TBTC) were more than 95% and about 3%, respectively.

Determination of tributyltin compounds in fish and shell-fish by GC using electron capture detector.

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