電子捕獲型検出器付きガスクロマトグラフィー又はガスクロマトグラフィー質量分析法による魚類中のトリブチルスズ化合物の定量

抄録

Gas chromatographic methods with ⁶³Ni electron capture detection (GC-ECD) or mass spectrometry (selected ion monitoring, SIM) was investigated for the determination of tributyltin compounds in fish. Tributyltin compounds in a homogenized flesh sample of fish were extracted as tributyltin chloride (TBTC) with a hydrochloric acid-methanol mixture and transferred to a hexane solution. The extract was charged to an alumina column and eluted stepwise with ethyl acetate followed by hexane-ethanol (4 : 1, v/v) mixture. TBTC eluted with the latter solvent was transferred to a hexane layer by liquid-liquid extraction, and the hexane layer was concentrated by a rotary evaporator. The concentrate was subjected to gas chromatographic separation on a 10% KOCL-Sn column. The calibration curves were linear in the range of 0.1-2 μg/ml with GC-ECD and in the range of 0.05-1 μg/ml with SIM, respectively. The detection limit of TBTC was 0.005 μg/g in sample by the SIM method. Eleven samples of fish were analyzed by the GC-ECD and SIM methods, and the determined values by both the methods were in good agreement.