杜建业, 臧鳳和, 吴兆汉, 吴锦健. 枸橼酸小蘗碱的制备及其分析方法的研究J. 药学学报, 1963, 10(2): 91-96.
引用本文: 杜建业, 臧鳳和, 吴兆汉, 吴锦健. 枸橼酸小蘗碱的制备及其分析方法的研究J. 药学学报, 1963, 10(2): 91-96.
TU CHIEN-YEH, TSANG FENG-HO, Wu CHAO-HAN AND WU CHIN-CHIEN, . BERBERINE CITRATE, ITS PREPARATION AND ANALYSISJ. Acta Pharmaceutica Sinica, 1963, 10(2): 91-96.
Citation: TU CHIEN-YEH, TSANG FENG-HO, Wu CHAO-HAN AND WU CHIN-CHIEN, . BERBERINE CITRATE, ITS PREPARATION AND ANALYSISJ. Acta Pharmaceutica Sinica, 1963, 10(2): 91-96.

枸橼酸小蘗碱的制备及其分析方法的研究

BERBERINE CITRATE, ITS PREPARATION AND ANALYSIS

  • 摘要: 本文敘述了三个制备枸橼酸小蘗碱的方法,后二法可用于大量生产,第三法原則也适用于硫酸小蘗碱的制备。此外对于它的精制問題、物理化学性貭、分析測定等也作了詳細的介紹。

     

    Abstract: Three methods for the preparation of berberine citrate are described. (1) About 100 g of berberine hydrochloride and 200 ml of water were shaken together, and 300 ml of 30% NaOH was added; shaking was continued until the colour of crystal was obviously changed. The mixture was allowed to stand for a short time; the supernatant should be colourless. Then the free base was collected by filtration,washed with water until free from NaOH and then with a little alcohol. The ppt. was transferred into another bottle, 11 of alcohol and 120—150 g of citric acid were added. The mixture was refluxed until complete dissolution; after cooling, the crude product was collected in a Buchner funnel, and recrystallized from 70% alcohol. The yield is about60—70%. (2) About 100 g of berberine hydrochloride, 100 ml of acetone, and 400 ml H2O. Were heated together to 60—70℃, and with shaking, 50 ml of 50% NaOH was added. The mixture was kept at this temperature for 1—2 hours, cooled, and the berberineacetone was collected in a Buchner funnel, washed with water until the washings was colourless. The ppt. was transferred into a 21 bottle, 1500 ml 70% alcohol and 70 g of citric acid were added. The mixture was refluxed until complete dissolution, cooled, and the product was collected and purified from 70% alcohol. The yield is 85—95%. The berbetine citrate obtained is in pale yellow needles, m.p. 209—211℃. (3) About 1 kg of berberine hydrochloride was added to 12 liter of 70% alcohol and 1.2—1.5 kg citric acid. The mixture was Heated to boiling and 500 ml of 50% sodium hydroxide was added. It was kept at this temperature for 1—2 hours. After cooling, the crystalline product was collected and purified from 70% alcohol. The yield is 85—90%. The method can also be adapted for the preparation of berbetine sulphate from its hydrochloride. Two methods for the assay of berberine citrate are also described.

     

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