高效液相制备色谱制备土贝母中土贝母苷甲、乙、丙对照品的研究
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摘要
目的研究高效液相制备色谱从土贝母中制备土贝母苷甲、乙、丙对照品。方法采用大孔吸附树脂和制备液相色谱等多种方法进行分离纯化,并根据理化性质和波谱数据鉴定化合物的结构。结果分离得到3个化合物,分别鉴定为土贝母苷甲、土贝母苷乙、土贝母苷丙,收率分别为0.58%、0.13%、0.13%,HPLC归一化法测得质量分数均大于98%。结论本方法上样量大,重现性好,收率高,适合土贝母苷甲、乙、丙的大量制备生产。
Objective To study the preparation technology of tubeimosides I, II, and III reference substances from Bolbostemma paniculatum by preparative HPLC. Methods Chemical constituents were isolated and purified by macroporous adsorption resin and preparative high performance liquid chromatography. Their structures were identified on the basis of physicochemical properties and spectroscopic data. Results Three compounds were isolated and they were identified as tubeimosides I, II, and III. The yields were 0.58%, 0.13%, and 0.13%. And the purity detected by HPLC was above 98%. Conclusion The method has the advantages of large samples and good repeatability. It can be applied to large-scale preparation of tubeimosides I, II, and III.
Objective To study the preparation technology of tubeimosides I, II, and III reference substances from Bolbostemma paniculatum by preparative HPLC. Methods Chemical constituents were isolated and purified by macroporous adsorption resin and preparative high performance liquid chromatography. Their structures were identified on the basis of physicochemical properties and spectroscopic data. Results Three compounds were isolated and they were identified as tubeimosides I, II, and III. The yields were 0.58%, 0.13%, and 0.13%. And the purity detected by HPLC was above 98%. Conclusion The method has the advantages of large samples and good repeatability. It can be applied to large-scale preparation of tubeimosides I, II, and III.
引文
[1]中国药典[S].一部.2010:18-19.
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[2]马挺军,李军,屠鹏飞,等.土贝母中一个新的三萜皂苷[J].中草药,2006,37(3):327-329
[3]孔凡华,朱大元,徐任生,等.土贝母化学成分的研究(III)土贝母甙甲的结构[J].化学学报,1988,46(8):772-778.
[4]孔凡华,朱大元,徐任生,等.土贝母化学成分的研究(Ⅳ)土贝母甙乙、丙、丁的结构[J].化学学报,1988,46(4):409-411.
[5]Kasai R,Miyakoshi M,Nie R L,et al.Saponins from Bolbostemma paniculatum:cyclic bisdesmosides,tubeimosides II and III[J].Phytochemistry,1988,27(5):1439-1446.