洋地黄叶的分析——Ⅱ.薄层层离测定

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洋地黄叶提出物在甲酰胺作固定相的硅藻土薄层上,用氯仿-丙酮-醋酸乙酯-乙醇-甲酰胺(8∶2∶0.5∶0.5∶饱和),或氯仿-丁醇-甲酰胺(9∶1∶饱和),或氯仿-醋酸乙酯-苯-甲酰胺(1∶3∶2∶饱和)作展开剂,分别分离毛花洋地黄一级甙,紫花洋地黄一级甙,或二级甙。展开后的板,于100℃烤去甲酰胺,碘蒸气显点,用吸取器将色点吸下,以呫吨氢醇的冰醋酸溶液洗脫。洗脫液中加入一定量盐酸后,显色测定。曾测定了六种纯强心甙的回收率,除羟基洋地黄毒甙因色点有拖尾,结果偏低,为87.7%外;毛花洋地黄甙甲、乙、丙,洋地黄毒甙,异羟基洋地黄毒甙等的回收率均在94.9—97.6%间,标准偏差0.6—2.6%。用本法测定了毛花洋地黄及紫花洋地黄二种干叶中的主要强心甙含量,结果与纸层离法基本一致,但本法操作时间可以大大缩短,误差小,而且也容易掌握。 Digitalis leaf extract on a thin layer of diatomaceous earth with formamide as the stationary phase using chloroform-acetone-ethyl acetate-ethanol-formamide (8:2:0.5:0.5:saturated), or chloroform-butanol- Carboxamide (9:1:saturated), or chloroform-ethyl acetate-benzene-carboxamide (1:3:2:saturated) as developing solvent, were used to separate the first-class alfalfa of F. purpurea and the first-class alfalfa of D. Or two levels. The developed plate was baked at 100°C to formamide, and the iodine vapor was visualized. The color spot was sucked off with a suction device and eluted with a solution of xanthene alcohol in glacial acetic acid. After a certain amount of hydrochloric acid was added to the eluate, the color was measured. The recovery rates of six kinds of pure cardiac palpitations were determined, except for the oxytodix drug glycoside with tailing due to the color point, and the result was low, which was 87.7%; the virgin glycosides were glycosides, B, C, and digoxigenin. The recoveries of aredoxitol and digoxigenin were between 94.9 and 97.6% with a standard deviation of 0.6 to 2.6%. The main cardiotonin levels in the two dry leaves of F. purpurea and D. intermedium were determined by this method. The results were basically consistent with the paper delamination method. However, this method can greatly shorten the operation time, have a small error, and it is easy to grasp. .
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