Comparison of various analytical methods for determination of total and ionic fluoride in biological samples.

为寻找一种测定生物样品中总氟和离子氟的合适方法，采用了6种分析方法：氟离子选择电极法(IE法)、微扩散气相色谱(DIF-GC法)、AlF分子吸收光谱法(AlF法)、低温灰化-GC法(LTA-GC法)，而热解-GC(PYH-GC法)和直接萃取-GC(DE-GC法)是本研究的新方法。考察了PYH仪器的操作条件和小牛血清回收氟的方法。此外，还用DE-GC法测定了给予有机氟化合物的大鼠硬组织中的离子氟。对上述方法进行了检验，将其中一些方法结合起来测定了不同样品中的总氟和离子氟；所用的样品是含有机氟化合物的样品和含…的大鼠组织更多的CH被给予了地氟尼特。结果如下：1.用四种分析方法测定了六种有机氟化合物的回收率。在四种测定方法的比较中，使用强酸的DIF-GC法被证明是不足的，而AlF法对一半被检测的有机F化合物的回收率很低。虽然PYH-GC法对熔点低的对氟二苯甲酮的回收率较低，但对其他有机氟化合物的回收率较高，LTA-GC法的回收率最高。2.经LTA和PYH处理的大鼠血浆和软组织的总F值与经LTA和PYH处理的大鼠血浆和软组织中的总F值具有很好的一致性。结果表明，两种方法均适用于血浆和软组织中氟及其代谢物的测定。但由于PYH-GC法比LTA-GC法更快速、更简便，因此用PYH-GC法测定生物样品中总氟效果更好。3.DIF-GC法与DE-GC法测定大鼠硬组织中的离子氟具有良好的一致性。从这一结果来看，DE-GC方法比DIF-GC方法更可取，因为它非常简单和快速。较少

The objective of this study was to find a suitable method for the determination of total and ionic fluoride(F) in biological samples.Six procedures were employed for the fluoride analysis; the fluoride ion selective electrode (IE method), the microdiffusion-gas chromatography (Dif -GC method), AlF molecular absorption spectrometry (AlF method), the low temperature ashing-GC (LTA-GC method) had previously been reported, while the pyrohydrolysis-GC (PyH-GC method) and the direct extraction-GC (DE-GC method) were newly applied to this study.We investigated the operating conditions of the apparatus for PyH and the recovery of F using calf serum. In addition, the DE-GC method was applied to determine ionic F in the hard tissues of rats which had been given Diflunisal (organic F compound).The above mentioned methods were tested by combining some of them for determining total and ionic F in various samples; the samples used were those containing organic F compounds and the tissues of rats whi … More ch had been given Diflunital. The F values obtained were then compared.The results were as follows: 1. The recovery rates of six organic F compounds were measured by four analytical methods. In comparing the four determining methods, the Dif-GC method using a strong acid proved to be deficient and the AlF 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. 2. The total F values in the plasma and soft tissues of 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 Diflunisal and its metabolite in the plasma and soft tissues. However, it is better to use the PyH-GC method for determination of total F in biological samples because it is more rapid and simpler than the LTA-GC method. 3. The ionic F in the hard tissues of rats showed good agreement between the samples determined by the Dif-GC and the DE-GC method. From this result, the DE-GC method is preferable to the Dif-GC method because it is very simple and rapid. Less