著者

甲斐 雅亮 三浦 哲朗 小橋 一弥 大倉 洋甫

出版者

The Pharmaceutical Society of Japan

雑誌

Chemical and Pharmaceutical Bulletin (ISSN:00092363)

巻号頁・発行日

vol.29, no.4, pp.1115-1120, 1981-04-25 (Released:2008-03-31)

参考文献数

16

被引用文献数

31 32

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A new fluorimetric method for the precise and rapid determination of guanidino compounds with benzoin is described. This is based on their reaction in an aqueous potassium hydroxide solution with benzoin (dissolved in methylcellosolve), in the presence of β-mercaptoethanol and sodium sulfite, while the pH of the reaction mixture is maintained at 9.2 after the reaction. This method requires heating at 100° for only 10 min. The excitation and emission maximum wavelengths of the fluorescence from these compounds are at around 325 and 435 nm, respectively. The method is simple, selective for guanidine and monosubstituted guanidino compounds (including peptides with one or two arginyl residues) and sensitive ; almost all the compounds can be determined at concentrations as low as 40-170 pmol/ml.

著者

甲斐 雅亮 坂本 靖浩 三浦 哲朗 大倉 洋甫

出版者

公益社団法人 日本分析化学会

雑誌

分析化学 (ISSN:05251931)

巻号頁・発行日

vol.35, no.3, pp.329-332, 1986-03-05 (Released:2009-06-30)

参考文献数

7

被引用文献数

2 2

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A high performance liquid chromatographic method is described for the determination of antipain which is a protease inhibitor and also a possible therapeutic drug for muscular destrophy. Antipain was converted to the fluorescent derivative by reaction with benzoin, a fluorogenic reagent for guanidino group. The derivative was then determined on a reversed phase column with isocratic elution within 15 min by using fluorescence detector. The detection limit of antipain in mouse serum was 0.42μg/ml, which corresponds to the amount of 240 pg (400 fmol) in an injection volume of 100μ1 at a signal to noise ratio of 2. The calibration graph for the compound was linear up to at least a concentration of 30 μg/ml in the serum. The proposed method was simple, rapid and sensitive enough to permit the quantification of antipain in as little as 40 μl of mouse serum dosed with the compound.

著者

西岡 五夫 松尾 律子 大倉 洋甫 百瀬 勉

出版者

公益社団法人日本薬学会

雑誌

薬学雑誌 (ISSN:00316903)

巻号頁・発行日

vol.88, no.10, pp.1281-1285, 1968-10

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A new colorimetric method for microdetermination of isothiocyanates was established, using 3,6-dinitrophthalic acid as a color developing agent in a potassium carbonatesodium thiosulfate solution. The reaction conditions were examined with allyl isothiocyanate as a model compound. The outline of the procedure is as follows : To 2.0 ml of allyl isothiocyanate solution (10-150 μg/ml), (dissolved in 50% ethylene glycol solution, 1.0 ml of 3,6-dinitrophthalic acid monopyridinium salt solution (0.1%), and 1.0 ml of alkaline solution (40% potassium carbonate and 30% sodium thiosulfate) are added and mixed well. The mixture is heated in a boiling water bath for exactly 10 minutes, cooled in running water, and diluted to 20.0 ml with water. The absorbance of the developed color is read at 400 mμ against the reagent blank. In this color reaction, 3,6-dinitrophthalic acid was assumed to be reduced to 3-amino-6-nitrophthalic acid by S^<2->, which was liberated from allyl isothiocyanate in the alkaline medium.