o-アミノチオフェノールによるけい光分析(第2報) : 塩酸トンジルアミンのけい光定量
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概要
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Fluorometric determination of thonzylamine hydrochloride (I) with o-aminothiophenol (II) was investigated. Previous to the determination of I, determination of p-anisaldehyde (III) with II was devised. The reaction for the determination of I involved the oxidation of I by NaIO_4 to produce III and fluorescence reaction of III with II. The fluorescent substance formed by this reaction was found to be 2-(4-methoxyphenyl) benzothiazole (IV) from its spectroscopic and fluorometric analysis. Fluorescence characteristics of IV in various media were examined, and it was found that IV exhibited the strongest fluorescence in an acid solution of pH below 0.35. Based on this fact, fluorometric determination of III and I with II was established. The recommended analytical procedure for I is as follows : To 5 ml of a sample solution containing 0.5-50 μg of I, 5 ml of 10% (w/v) Na_2CO_3 and 0.5 ml of 0.1% NaIO_4 are added, warmed for 15 minutes in a boiling water bath, and the reaction product is extracted with 10 ml of ether. The ether layer is washed twice with 5 ml of water, 1 ml of 0.5% II-hydrochloride is added, ether is evaporated, and 5 ml of 30% (w/v) H_2SO_4 is added to the residue. The mixture is heated for 1 hour, cooled, diluted to 20 ml with water, and the fluorescence of this solution with the maximum 412 mμ is measured. By this method, 0.1-10 μg of I per ml can be determined. Procedure for the determination of III is identical with the reaction of oxidation product of I with II in the procedure for I, and 0.1-1.0 μg of III per ml can be determined.
- 公益社団法人日本薬学会の論文
- 1972-04-25
著者
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