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麦角新鹼的层离及提取的研究
引用本文:周同惠.麦角新鹼的层离及提取的研究[J].药学学报,1957,5(2):143-149.
作者姓名:周同惠
作者单位:中国医学科学院药物系分析室
摘    要:麦角为极常用的产科药物,其中所含生物鹼据文献中报告一般常见者有六对之多,而以水溶性之麦角新鹼效力最好,毒性最小.自Foster等发表用纸层离法鉴定麦角新鹼以后,才有了比较好的定性试验以肯定麦角新鹼的存在与否,但是这个方法至少需要十六到十八小时才能得到结果,时间上很不经济,因此有必要寻找一个比较快的方法.根据Brindle等用纸层离分离水不溶性生物鹼的结果,著者试用了含有缓的纸进行水溶性生物鹼的层离,用氯仿为推进剂,得到满意结果,不但麦角新鹼斑

收稿时间:1957-02-13

CHROMATOGRAPHIC SEPARATION AND EXTRACTION OF ERGONOVINE
CHOW TUNG-WHEI.CHROMATOGRAPHIC SEPARATION AND EXTRACTION OF ERGONOVINE[J].Acta Pharmaceutica Sinica,1957,5(2):143-149.
Authors:CHOW TUNG-WHEI
Abstract:Use was made of buffer-impregnated paper for the separation and indentifica- tion of ergonovine from other ergot alkaloids. It was found that the Rf value of ergonovine depends on the pH value of the buffer used. Paper moistened with a mixture of pH 7 buffer solution, acetone and formamide (2:2:1) gave good results with chloroform as developer. The separation was good and the spots were well defined. It took only about 2 hours to develop the chromatogram. Since the Rf value varies with temperature, amount of aqueous phase on the paper, etc., it is suggested that pure alkaloid be run at the same time as the sample for identifica- tion purpose. The partition chromatography of ergonovine, ergometrinine, ergotoxine and lysergic acid on a celite column with buffer solutions of various pH values was also studied in order to find optimal conditions for the extraction of ergonovine from ergot. With a pH 3.4 buffer solution, lysergic acid and ergonovine stayed on the top of the column while other alkaloids moved down. When the column was eluted with ammonia-saturated chloroform, ergonovine was washed out, thus separated from lysergic acid. From these results, pure ergonovine maleate crystals were obtained from ergot by the following proposed method: Prepare a chromatographic column of celite containing pH 3.4 buffer solution. Extract alkaloids from ergot with chloroform containing methanol and ammonia, acidify the extract to pH 3.4 with 2 N sulfuric acid in ethyl acetate solution. Run this mixture through the column. Ergonovine will stay adsorbed. Elute the column with ammonia-saturated chloroform, distil off the organic solvent under reduced pressure, cool, filter, dissolve the residue in acetone, add a solution of malefic acid in acetone; ergonovine maleate will separate out as pure, white crystals.
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