DETERMINATION OF 2,2,2-TRICHLOROETHANOL IN PLASMA AND URINE BY ION-EXCLUSION CHROMATOGRAPHY

被引:2
作者
ITOH, H
IKEDA, S
ICHINOSE, N
机构
[1] RYUKOKU UNIV, SCI & TECHNOL RES INST, FUSHIMI, KYOTO 612, JAPAN
[2] HAMAMATSU UNIV SCH MED, HAMAMATSU, SHIZUOKA 43131, JAPAN
关键词
2,2,2-TRICHLOROETHANOL; BETA-GLUCURONIDASE; PLASMA; URINE; ION-EXCLUSION CHROMATOGRAPHY;
D O I
10.1039/an9941900409
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
A simple and rapid chromatographic method has been developed for the determination of 2,2,2-trichloroethanol (TCEOH) and its glucuronide in plasma and urine. A glass column (150 x 6.6 mm i.d.) packed with Aminex A-5 cation-exchange resin (potassium form) following the slurry method was used as the analytical column, and an admixture or 10 mmol l-1 potassium sulfate and 10 mmol l-1 potassium hydroxide solution as the eluent (pH 12.2). Diluted plasma samples and urine samples were directly injected into the chromatograph through a 0.45 mum membrane filter without deproteinization. The amount of TCEOH conjugated to glucuronide was determined following treatment with beta-glucuronidase (200 U) for 30 min at 37-degrees-C. This allowed the concentration of free, total, and conjugated TCEOH to be determined. The calibration graph was rectilinear from 5 to 500 mg 1-1 of TCEOH, with a detection limit of 3 mg l-1, 2sigma, being the signal-to-noise ratio. The analytical recovery of TCEOH, obtained by analysing spiked plasma and urine samples, was in the range 98.4-102% and the relative standard deviation was less than 3.5%.
引用
收藏
页码:409 / 413
页数:5
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