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目的:对异型南五味子根茎中的倍半萜类化合物进行分离、结构鉴定和细胞毒活性研究。方法:将药材异型南五味子根茎阴干,粉碎成粗粉,用95%乙醇提取3次,每次1 h。减压回收提取液至无醇味后,将提取液用水分散,过聚酰胺柱色谱,依次用不同体积分数乙醇洗脱,得到水洗脱物,30%乙醇洗脱物,60%乙醇洗脱物和95%乙醇洗脱物。30%乙醇洗脱部位过小孔树脂柱色谱(MIC),不同体积分数乙醇洗脱MCI树脂,得到水洗脱物,30%乙醇洗脱物,50%乙醇洗脱物和95%乙醇洗脱物,50%乙醇洗脱物为富集得到的总倍半萜部位。以甲醇-水为流动相,用中压制备液相色谱对总倍半萜类部位进行分离,用TLC和HPLC对得到的组分进行合并。对于含有倍半萜的组分用高效液相色谱进行分离,分离得到单体化合物。得到的单体化合物用ESI-MS和NMR谱学技术进行结构确定。结果:从异型南五味子根茎中获得8个倍半萜类化合物,结构分别鉴定为1α-hydroxy-9-deoxycacalol(1),balsamiferine B(2),balsamiferine D(3),chaetopenoid A(4),chaetopenoid B(5),asterothamnone A(6),asterothamnone B(7),and 10-dehydroxy-melleoliede B(8)。体外抗肿瘤活性筛选表明,化合物2,6,7对人肝癌细胞(SMMC7721)具有抑制活性,半数抑制浓度分别为10.6,9.5和15.5μmol·L~(-1)。结论:倍半萜化合物1~8为从南五味子属植物中首次获得。
OBJECTIVE: To study the separation, structure identification and cytotoxicity of sesquiterpenoids in the rhizomes of Schisandra chinensis. Methods: Radix kadsura rhizome dry, crushed into meal, extracted with 95% ethanol three times, each time 1 h. After the extract was extracted under reduced pressure to give no alcoholic taste, the extract was dispersed with water, passed through a polyamide column and eluted with different volume fractions of ethanol to obtain water eluate, 30% ethanol eluate and 60% ethanol And 95% ethanol eluate. The column was eluted with 30% ethanol and the MCI resin was eluted with different volume fractions of ethanol to obtain water eluate, 30% ethanol eluate, 50% ethanol eluate and 95% ethanol The 50% ethanol eluate is the total sesquiterpene fraction enriched. With methanol-water as mobile phase, the total sesquiterpene fractions were separated by medium pressure preparative liquid chromatography and the fractions were combined by TLC and HPLC. For the sesquiterpene-containing components by high performance liquid chromatography separation, isolated monomer compounds. The resulting monomer compounds were confirmed by ESI-MS and NMR spectroscopy. Results: Eight sesquiterpenes were obtained from the rhizomes of the different genus Schisandra chinensis. The structures were identified as 1α-hydroxy-9-deoxycacalol (1), balsamiferine B (2), balsamiferine D (3), chaetopenoid A chaetopenoid B (5), asterothamnone A (6), asterothamnone B (7), and 10-dehydroxymelleoliede B (8). In vitro anti-tumor activity screening showed that compounds 2,6,7 have inhibitory activity against human hepatocellular carcinoma cells (SMMC7721), with median inhibitory concentrations of 10.6, 9.5 and 15.5μmol·L -1, respectively. Conclusion: Sesquiterpene compounds 1 ~ 8 were obtained from the genus Kadsura for the first time.