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[摘要]
目的研究制备型高效液相色谱Pep-HPLC分离纯化荷叶碱的方法。结论荷叶提取物经1%盐酸水溶液提取后,用氯仿萃取。萃取液蒸干,以流动相溶解。用P rep-HPLC分离制备。收集液浓缩到一定体积析出针状晶体,即得荷叶碱。结果该方法所得产品经M S、IR、UV1、H-NM R和HPLC图谱鉴定,与文献、对照品比较,确定为荷叶碱,质量分数大于98%,制备收得率大于49%。结论本法生产周期短,产品质量高,方法简便,生产费用低,荷叶碱产品可以用作分析方法的对照品。
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[Abstract]
Objective To study the solubility of lipo-alkaloids from prepared aconite root(Radix Aconiti Lateralis Preparata) and identify the sources of lipo-alkaloids in Sini Decoction.Methods The electrospray ionization mass spectrometry was employed to analyze the alkaloids in crude aconite roots,Sini Decoction,the gruffs of concocted aconite roots and the decoction of prepared aconite root and pinellia tuber(Rhizoma Pinellae).Results Lipo-alkaloids were observed in Sini Decoction,however,no lipo-(alkaloids) were found in the decoction of aconite roots with pinellia tuber.Lipo-alkaloids were the dominant components in the gruffs of concocted aconite roots.Conclusion Lipo-alkaloids are barely soluble in boiling water.The alkaloids existed in the Sini Decoction stem from the ester-exchange reactions of diester-diterpenoid alkaloids and fatty acid in the boiling water
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[基金项目]
国家“十五”重大专项“创新药物及中药现代化”“食品安全关键技术”;湖南省杰出青年基金资助项目(03JJY1002,2001BA746C,2001BA804A21,2003AA2Z3515)