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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 methyl esterification by methanol, and TCE was measured with decomposition of conjugation adding sulfuric acid. (1) As preliminary treatment, 0.1 ml of urine and 0.6 ml 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%, 0.001-0.783 mg/l and 0.8-4.0%, respectively, while those of TCE were 98.6-102.5%, 0.024-1.603 mg/l and 0.8-4.0%, respectively. (3) Calibration curves were linear up to 30 mg/l for TCA (y = 1.838x + 0.023, r = 0.999, n = 8) and 60 mg/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 less than 0.001) and TCA (y = 0.891x - 2.36, r = 0.928, n = 100, p less than 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 0.002 mg/l for TCA and 0.005 mg/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.

Determination of trichloroacetic acid and trichloroethanol by head-space gas chromatography(HSGC).