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抄録
環境中水にμg/lレベルで存在する2,4,6-トリアミノ-1,3-5-トリアジン(慣用名:メラミン)を活性炭カラムで抽出し,トリフルオロ酢酸を触媒として,N,O-ビス(トリメチルシリル)トリフルオロアセトアミドを用いてシリル化の後,ガスクロマトグラフ質量分析計により定量する方法を検討した.本法により,河川水や水道水更には塩を多量に含む海水からも微量のメラミンを定量的に抽出し分析することができた.本法によるメラミンの回収率は,1μg/lの濃度で97.7%であり,その相対標準偏差は4.9%であった.本法を用いて実際の海水,河川水及び水遠水を分析した結果,ほとんどの検体からメラミンが検出され,環境中に広く拡散,残留していることを確認した.
Determination of trace melamine (2,4,6-triamino-1,3,5-triazine) in water was developed for investigating the fate of melamine in environmental water samples. A water sample (500 ml) was passed through artificial activated carbon column (spherical beads, 20〜30 mesh, 0.5 cm i. d.×10 cm), after the sample had been passed through SEP-PAC[○!R] C_<18> for elimination of other contaminants. Melamine adsorbed on the activated carbon was extracted in a Soxhlet extractor with methanol for 4 h. The extract was concentrated to a few milliliters. The concentrate was transferred to a reactivial and dried at 80℃ under a stream of nitrogen. For the derivatization of melamine, 100 μl of trifluoroacetic acid and 600 μl of N,O-bis(trimethylsilyl)trifluoro-acetamide was added to the residue, and the mixture was heated at 100℃ for 10 min. After cooling, the reactant was examined by a gas chromatograph mass spectrometer with a selected ion detector (GC/MS-SID, m/z 342 and 327). In order to determine the accuracy and the precision of this method, 0.5 μg of melamine was added to 500 ml of purified water, river water and seawater and over-all recovery tests were performed. The average recovered amount of melamine was 0.49 μg and the standard deviation was 0.024 μg. By this method, river water, seawater and tapwater were analyzed and melamine was detected at 0.20〜0.72, 0.05〜0.07 and 0.05 μg/l, respectively.
