交流ポーラログラフィーによるワルファリンの定量
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概要
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Warfarin, 3-(α-acetonylbenzyl)-4-hydroxycoumarin, a rodenticide, showed a well-defined a. c. polarographic wave in sodium acetate-acetic acid solution, and it was applied to a simple, rapid, and precise determination of Warfarin. The recommended procedure is as follows. About 1mg of Warfarin is dissolved in 5m<I>l</I> of glacial acetic acid and to it is added 7m<I>l</I> of 5<I>M</I> sodium hydroxide solution. After deaeration with nitrogen, a. c. polarogram is recorded.<BR>Warfarin did not give d. c. polarographic wave in this solution. The peak potential of a. c. polarogram in sodium acetate-acetic acid solution was <I>ca</I>.-1.25V <I>vs</I>. S. C. E. The a. c. polarographic wave could be seen on 8×10<SUP>-5</SUP><I>M</I> Warfarin solution. It was seen that Warfarin was adsorbed on the electrode in the more negative potential range than the electrocapillary curve maximum potential (Fig. 1). The relation between the desorption potential and the concentration of Warfarin conformed to the equation (<I>E</I><SUB>T</SUB>-<I>E</I><SUB>e. m. c</SUB>.)<SUP>2</SUP> = (ln <I>C</I>+ln <I>K</I><SUB>a.o</SUB>. /<I>K</I><SUB>d.o</SUB>.)/ (α '+β '), which Breyer has introduced with respect to tensammetric wave (Fig. 6).<BR>Warfarin within the concentration range of 8×10<SUP>-5</SUP>5.4×10<SUP>-4</SUP><I>M</I> gave a linear relationship between the peak height and concentration in sodium acetateacetic acid supporting electrolyte solution. From its peak height, about 80μg/m<I>l</I> of Warfarin could be determined. The coefficient of variation was 1.10%, and the average recovery was 100.21% (Table II).
- 社団法人 日本分析化学会の論文
著者
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上田 嘉彦
大正製薬株式会社大宮工場品質管理部試験課
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森下 淑郎
大正製薬株式会社大宮工場品質管理部試験課
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小村 忠之
大正製薬株式会社大宮工場品質管理部試験課
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相川 千枝
大正製薬株式会社大宮工場品質管理部試験課