ヘッドスペース・ガスクロマトグラフィーによる臓器中クロロホルムの定量 : 均質な試料の調製法

抄録

The present study was focused on the preparation of a homogeneous sample solution for the determination of chloroform in the tissue of brain or lung of a rabbit. Into a pair of vial (7 ml) both of 200 mg of brain sample and 0.4 ml of 10% (v/v) Triton X-100 in water were taken, and adjusted to a total volume of 0.8 ml with water. Each vial was sealed with a screw-cap with a septum lid. The sample mixture was irradiated by ultrasonic wave (20 KC, 100 W) for 5 min under cooling on running water. Into the resulting duplicate tissue homogenate samples was injected 200 μl of either one of standard sample solutions, (a) or (b) through the septum lid : (a), 20% methanol solution (200 μl) containing 30 μg of CHCl₃ and 20 μg of CH₃CCl₃ (internal standard) ; (b), the same solution containing 15 μg of CHCl₃ and 20 μg of CH₃CCl₃. The both vials were allowed to stand for 15 min at 65°C on a heating block. A portion (400 μl) of the headspace gas was analyzed by GC with a flame ionization detector. GC conditions used were as follows : Glass column (1.6 m×3 mm i.d.) packed with Chromosorb 102 (80-100 mesh) ; Column oven, 170°C ; Detector and injector temperatures, 220°C ; Carrier gas, N₂ 50 ml/min. In the case of lung tissue sample, the mixture was incubated at 35°C for 2 h in the presence of collagenase in the sealed vial prior to the sonication. The successive experimental mannuals were mostly the same as those of the brain. The present headspace GC was found to be reliable for the determination of CHCl₃ in a range of 2 to 40 μg/ml in the homogeneous sample solution.