シクラミン酸塩の螢光法による加水分解率測定

概要

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A fluorometric determination of cyclohexylamine by the use of 5-dimethylaminonaph thalene-1-sulfonyl chloride (DNS-Cl) was devised. The recommended analytical procedure is as follows : to 2 ml of a sample solution (0.087-17.4 mM), 1 ml of saturated sodium hydrogen carbonate solution, 4-5 ml of acetone, and 0.5-1.0 ml of 0.5% acetone solution of DNS-Cl are added successively. After standing for 7 hr at room temperature, the solution mixture is made to 10 ml with acetone. A definite volume (0.01-0.05 ml) of the reaction solution is spotted on a thin-layer chromatographic plate (Silica gel H : Avicel SF : soluble strarch=20 : 10 : 1) and developed with chloroform-pyridine mixture (20 : 1). A definite area of Rf 0.52 is scraped off and extracted with 10 ml of acetone. Fluorescence is measured at 497 mμ by the excitation light of 350 mμ. The reading of fluorescence intensity is referred to the 0.5 μg/ml solution of fluorescein sodium. Cyclohexylamine, the hydrolysis product of cyclamate under various conditions, was determined by this fluorometric method. Hydrolysis of two cyclamates in citric acid solution, citric acid and Sn^<2+> solution, acetic acid solution sodium nitrate solution, and sodium nitrate and sodium chloride solution is shown in Tables III and IV. Hydrolysis being very small under these conditions.
公益社団法人日本薬学会の論文
1971-05-25