综合运用正相和反相硅胶柱层析、Sephadex LH-20凝胶柱层析以及制备HPLC等分离方法,从1种中国南海海绵Xestospongia testudinaria中追踪分离抗肿瘤活性次级代谢产物。从95%乙醇提取物中分离获得8个单体化合物,通过NMR,MS等波谱技术鉴定其结构分别为:E-18,18-二溴-9,17-二烯-5,7-二炔硬脂酸甲酯(1),E-18,18-二溴-9,17-二烯-5,7-二炔硬脂酸乙酯(2),麦角甾-5,7,22-三烯-3-醇(3),麦角甾-4,6,8(14),22-四烯-3-酮(4),胆甾-4-烯-3-酮(5),3-吲哚醛(6),3-吲哚酸(7)和5-吲哚醛(8)。其中,化合物2-5和8为首次从该属海绵中分离得到。化合物1对肿瘤细胞株HCT116和A549显示较强的抑制活性。
The chemical constituents of sponge Xestospongia testudinaria from the South China Sea were investigated by bioassay-guided fractionation.Eight compounds were isolated from 95% ethanolic extract by repeated column chromatography on silica gel and Sephadex LH-20,and preparative-HPLC.By means of spectroscopic data including NMR and MS,their structures were elucidated as E-9,17-octadecadiene-5,7-diynoic acid-18,18-dibromo-methyl ester(1),E-9,17-octadecadiene-5,7-diynoic acid-18,18-dibromo-ethyl ester(2),ergosta-5,7,22-trien-3-ol(3),ergosta-4,6,8(14),22-tetraen-3-one(4),cholest-4-en-3-one(5),1H-indole-3-carboxaldehyde(6),1H-indole-3-carboxylic acid(7) and 1H-indole-5-carboxaldehyde(8).Compounds 2-5 and 8 were reported from genus Xestospongia for the first time.Moreover,compound 1 showed potent cytotoxicity towards tumor cell lines HCT116 and A549.