パイロハイドロリシス-ガスクロマトグラフィーによる生体試料中総フッ素定量の検討
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For determining the total fluorine (F) level in biological samples containing organofluorine (organic F) compounds, we used pyrohydrolytic F separation and gas chromatography for the determination of F in the resulting aqueous HF solution (PyH-GC method).<BR>We investigated the operating conditions of the apparatus for PyH which was developed by Itai et al. and the recovery of F using calf serum. In order to examine the suitability of the PyH-GC method for determining various organic F compounds, we applied four analytical methods including the PyH-GC method to test the recovery rates of six organic F compounds and then compared the F values obtained from each method.<BR>Furthermore, for confirming the applicability of the PyH-GC method to determine low level F in biological samples, we applied both the PyH-GC method and the low temperature plasma ashing method followed by GC (LTA-GC method) to determine the total F in the blood plasma of rats which had been given 6-fluoro-tryptophan (6-FT).<BR>The results were as follows:<BR>(1) Concerning pyrohydrolysis, the best results were obtained when the temperature of the steam generator was 95°C, sample quantities were 300μ<I>l</I> or 0.3-0.4g, and highly purified oxygen was used. When NaF, NH<SUB>4</SUB>F, 6-FT or CaF<SUB>2</SUB> was added to calf serum, good reproducibility and recovery rates were obtained without addition of any acid flux for total F determination. The detection limits in this method were 4ng/m<I>l</I> for serum and 3ng/g for soft tissue.<BR>(2) In comparing the four determining methods, the diffusion method using a strong acid proved to be deficient and the A<I>l</I>F molecular absorption method showed low recovery rates for half of the organic F compounds examined. Although the PyH-GC method showed a low recovery rate for 4-fluorobenzophenone which has a low melting point, it showed fairly good recovery rates for the other organic F compounds; the LTA-GC method showed the best recovery rate.<BR>(3) The total F values in the plasma of the rats resulted in an excellent agreement between the samples pretreated with LTA and those with PyH. This result indicates that both methods are suitable for determining F in 6-FT and its metabolite in the plasma.<BR>However, it is better to use the PyH-GC method for determination of total F in biological samples becausè it is more rapid and simpler than the LTA-GC method.
- 有限責任中間法人 日本口腔衛生学会の論文
有限責任中間法人 日本口腔衛生学会 | 論文
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