ガスクロマトグラフィー/質量分析法による水,底質中の1-ナフタレン酢酸の定量

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A method for the microdetermination of 1-naphthaleneacetic acid in environmental samples was developed. A water sample (11) was washed with hexane and extracted twice with 200 ml, and 100 ml of ethyl acetate. The extract was concentrated to dryness and 1 ml of diazomethane/ether solution was added to the residue for methylation. After removal of ether, the residue was dissolved in 1 ml of hexane. Silica-gel column chromatography was then carried out to remove interfering substances and 1-methylphenanthrene in samples. The hexane solution was placed on the top of a silica-gel (Wakogel C-200) column (1 cm×15 cm). The column was washed with 50 ml of hexane : benzene (1 : 1), and then 1-naphthaleneacetic acid methyl ester was eluted with hexane containing 10 % ether. After concentrating the eluate, 1-methylphenanthrene was added to the concentrate as an internal standard for analysis by gas chromatography mass spectrometry. In case of sediment, 20 ml of 1 M sodium hydroxide solution was added to 20 g of a sediment sample and mixed well. After ultrasonic extraction, the mixture was centrifuged and filtered. Then 20 ml of 1 M sodium hydroxide solution was added to the residue again and this procedure was repeated. All of the sodium hydroxide solutions was combined and washed with hexane, and the aqueous solution was acidified and extracted twice with 20 ml of ethyl acetate. The ethyl acetate layer was then treated in the similar way as water samples. Recovery of 1-naphthaleneacetic acid for water samples and sediment samples were 89 % and 75 %, respectively. Detection limits were 0.02 ppb and 1 ppb. This method was applied to some environmental samples, but 1-naphthaleneacetic acid was not detected in them.
社団法人日本分析化学会の論文
1985-07-05

ガスクロマトグラフィー/質量分析法による水,底質中の1-ナフタレン酢酸の定量

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