ヘッドスペース・ガスクロマトグラフ(HS・GC)法による尿中トリクロロ酢酸とトリクロロエタノールの分離定量

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Simultaneous determination of trichloroacetic acid (TCA) and trichloroethanol (TCE) in urine was made using head-space gas chromatography (HSGC). TCA was analyzed after methylesterification by methanol, and TCE was measured with decomposition of conjugation adding sulfuric acid. (1) As preliminary treatment, 0.1ml of urine and 0.6ml of esterizer (pure water: sulfuric acid: methanol=6: 5: 1, V/V/V) were mixed in a sample vial, which was sealed a septum. This was analyzed in HSGC. (2) By this method, the recovery, standard deviation and coefficient of variation of TCA were 95.7-104.3%, 0.001-0.783mg/l and 0.8-4.0%, respectively, while those of TCE were 98.6-102.5%, 0.024-1.603mg/l and 0.8-4.0%, respectively. (3) Calibration curves were linear up to 30mg/l for TCA (y=1.838x+0.023, r=0.999, n=8) and 60mg/l for TCE (y=0.963x+0.072, r=0.999, n=8). (4) A high correlation between HSGC and alkaline pyridine spectrophotometry was found for both TTC (TCA+TCE=TTC), (y=0.917x-3.08, r=0.980, n=100, p<0.001) and TCA (y=0.891x-2.36, r=0.928, n=100, p<0.001). The values for TCA and TCE obtained with HSGC were lower than those obtained with spectrophotometry. (5) The limits of the detection obtained with this method were 0.002mg/l for TCA and 0.005mg/l for TCE according to the formula recommended by International Union of Pure and Applied Chemistry (IUPAC). These results indicate that this simple method is accurate and useful in simultaneous detection of TCA and TCE.
社団法人日本産業衛生学会の論文
1991-03-20

ヘッドスペース・ガスクロマトグラフ(HS・GC)法による尿中トリクロロ酢酸とトリクロロエタノールの分離定量

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