梁彬, 周同惠. 麦角生物碱的层离研究——Ⅲ.麦角生药的纸层离定量J. 药学学报, 1963, 10(2): 87-90.
引用本文: 梁彬, 周同惠. 麦角生物碱的层离研究——Ⅲ.麦角生药的纸层离定量J. 药学学报, 1963, 10(2): 87-90.

麦角生物碱的层离研究——Ⅲ.麦角生药的纸层离定量

  • 摘要: 在以前的紙层离工作基础上,拟定出麦角新碱、麦角胺与麦角毒碱的紙层离定量方法。紙用緩冲液、甲酰胺、丙酮的混合液(2:1:1)处理,点上样品后以氯仿扩展。然后根据生物碱位置,或收集氯仿洗胱液,或用稀硫酸浸泡洗下,用对二甲氨基苯甲醛显色后定量。緩冲液之pH值对生物碱移动距离有影响,可改变之以达到不同測定目的。麦角胺与麦角毒碱的回收率分别为93.7%与94.4%。曾用此法分析麦角样品,結果与柱层离法相符合。

     

    Abstract: We reported previously the separation of ergot alkaloids by paper chromatographic method. The present paper deals with the quantitative determination of these alkaloids upon elution of the different spots and subsequent reaction with p-dimethylaminobenzaldehyde reagent. For the separate determination of ergonovine and total water-insoluble alkaloids, impregnate the paper with pH 4.4 buffer :formamide :acetone (2:1:1) mixture. Use chloroform as the developer, and let it run off the paper. Collect the organic phase in a small beaker beneath the paper, add 2 ml 0.2N H2SO4 and 4ml reagent, shake vigorously and determine colorimetrically the total water-insoluble alkaloid content. To determine ergonovine, cut off the paper holding this alkaloid, immerse in 2 ml 0.2 NH2SO4, stir well, add 4 ml reagent after 20 minutes and determine in the usual manner. For the determination of ergotamine and ergotoxine, the procedure was the same as above, except that a pH 2 buffer was used instead of pH 4.4. Ergotoxine ran off the paper while ergotamine remained on. Both were determined by treating with pdimethylaminobenzaldehyde solution as described above. The results were in agreement with those obtained by column chromatographic method. An unknown spot was found when pH 4.4 buffer was used; it also reacted with p-dimethylaminobenzaldehyde to a blue color. The Rf value was higher than that of ergonovine.

     

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