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Preparation of homogeneous sample solution for the determination of chloroform in tissue by headspace gas chromatography


Eisei Kagaku 34(2): 179-183
Preparation of homogeneous sample solution for the determination of chloroform in tissue by headspace gas chromatography
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) Trition 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 .mu.l of either one of standard sample solutions, (a) or (b) through the septum lid: (a), 20% methanol solution (200 .mu.l) containing 30 .mu.g of CHCl3 and 20 .mu.g of CH3CCl3 (internal standard); (b), the same solution containing 15 .mu.g of CHCl3 and 20 .mu.g of CH3CCl3. The both vials were allowed to stand for 15 min at 65.degree. C on a heating block. A portion (400 .mu.l) of the headspace gas was analyzed by GC with a flame ionization detector. GC conditions used were as follows: Glass column (1.6 m .times. 3 mm i.d.) peacked with Chromosorb 102 (80-100 mesh); Column oven, 170.degree. C; Detector and injector temperatures, 220.degree. C; Carrier gas, N2 50 ml/min. In the case of lung tissue sample, the mixture was incubated at 35.degree. C for 2 h in the presence of collagenase in the sealed vial prior to the sonication. The successive experimental manuals 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 .mu.g/ml in the homogeneous sample solution.


Accession: 006173254

DOI: 10.1248/jhs1956.34.179



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