Analysis of 1,4-Dimorpholino-7-phenylpyrido [3,4-d] pyridazine (DS-511) and Its Metabolites in Biological Specimens. III. Fluorodensitometric Method for the Simultaneous Determination of DS-511 and Its Metabolites in Urine and Bile

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概要

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• A simple and rapid fluorodensitometric method for the simultaneous determination of 1,4-dimorpholino-7-phenylpyrido [3,4-d] pyridazine (DS-511) and its metabolites in urine and bile was established. The biological specimens containing DS-511 and its metabolites were separated into lipophilic and hydrophilic layers by extraction with ethyl acetate. The hydrophilic layer was incubated at 37° for 24 hr with β-glucuronidase and arylsulfatase, then separated again into two layers by a similar extraction procedure. The lipophilic layers were purified by two-dimensional thin-layer chromatography with chloroform-methanol (10 : 1) and ethyl acetate-benzene (3 : 2). The hydrophilic layer was passed through a column of Amberlite XAD-2 (100-200 mesh), eluting with ethanol, and the eluate was purified by stepwise thin-layer chromatography with ethyl acetatebenzene (3 : 2) and chloroform-methanol (2 : 1). After moistening the air-dried chromatogram with 1-butanol, the fluorescent spots were quantitatively determined with a spectrodensitometer in the fluorescence mode. The recoveries and the coefficients of variation (c. v.) with this method were 89-116% (c. v. 6-14%) for lipophilic compounds and 93.0-95.0% (c. v. 5-6%) for hydrophilic compounds at concentrations between 0.1-1.0 μg/ml in biological specimens. This method could be used to analyze biological specimens from rats and dogs after administration of DS-511 and should also be applicable to human specimens.

• 公益社団法人日本薬学会の論文
• 1980-07-25

著者

• 西川 浩平

  Central Research Division, Takeda Chemical Industries, Ltd.,

• 三宅 荘八郎

  Central Research Division Takeda Chemical Industries Ltd.

• 桑山 素明

  Central Research Division, Takeda Chemical Industries, Ltd.

• 西川 浩平

  Central Research Divistion Takeda Chemical Industries Ltd.

• 桑山 素明

  Central Research Division Takeda Chemical Industries Ltd.

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• Analysis of 1,4-Dimorpholino-7-phenylpyrido [3,4-d] pyridazine (DS-511) and Its Metabolites in Biological Specimens. III. Fluorodensitometric Method for the Simultaneous Determination of DS-511 and Its Metabolites in Urine and Bile

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