论文部分内容阅读
目的:对夹竹桃科狗牙花属植物中狗牙花的生物碱类化学成分进行分离并对分离得到的化合物进行结构鉴定。方法:将干燥狗牙花3.5 kg粉碎,加甲醇室温渗漉提取,收集渗滤液,将渗滤液减压浓缩得到浸膏。浸膏用2 mol·L~(-1)硫酸调节p H 2,加入乙酸乙酯萃取得到非碱性脂溶性成分浓缩物;萃取后的酸水液用氢氧化钠溶液调节p H 9~10,然后用三氯甲烷萃取,得到总生物碱10 g。通过硅胶柱色谱,小孔凝胶(MCI)柱色谱和LH-20羟丙基萄聚糖凝胶(Sephadex LH-20)柱色谱进行分离和重结晶技术纯化,应用TLC监测,分离得到纯度较高的单体化合物。利用现代波谱法结合理化分析对其化学结构进行进一步鉴定。结果:从狗牙花中共分离得到并鉴定了6个单吲哚生物碱,分别鉴定为ervaramine型:ervatamine(1),20-epiervatamine(3);vobasine型:tabernaemontanine(2),dregamine(4);aspidosperma型:(-)-mehranine(5),tetrahydroalstonine(6)。结论:化合物4,6为首次从该植物中分离得到。MTS法测定化合物的肿瘤细胞毒活性,化合物1~6对5种人体肿瘤细胞株(人早幼粒白血病细胞HL-60,人肝癌细胞SMMC-7721,人肺癌细胞A-549,人乳腺癌细胞MCF-7,人结肠癌细胞SW-480)未显示出细胞毒活性。
OBJECTIVE: To separate the alkaloids of Apocynaceae from Apocynaceae of Apocynaceae and elucidate the structures of the isolated compounds. Methods: The dry dog tooth flower 3.5 kg crushed, add methanol percolation extraction at room temperature, the leachate collected, the leachate was concentrated under reduced pressure to give extract. The extract is adjusted to pH 2 with 2 mol·L -1 sulfuric acid and extracted with ethyl acetate to obtain a concentrate of non-alkaline fat-soluble ingredients; the extracted aqueous acid solution is adjusted to pH 9-10 with sodium hydroxide solution , Then extracted with trichloromethane to give a total alkaloid of 10 g. Purification by silica gel column chromatography, gel filtration (MCI) column chromatography and LH-20 hydroxypropyl dextran gel chromatography (Sephadex LH-20) column chromatography and recrystallization technology, TLC monitoring, isolated purity High monomeric compounds. The use of modern spectroscopy combined with physical and chemical analysis of its chemical structure to further identify. Results: Six single indole alkaloids were isolated and identified from erinaceus. They were identified as ervaramine type: ervatamine (1), 20-epiervatamine (3), vobasine type: tabernaemontanine (2) ; aspidosperma type: (-) - mehranine (5), tetrahydroalstonine (6). Conclusion: Compound 4,6 was isolated from this plant for the first time. Tumor cytotoxic activity of the compounds was determined by the MTS assay. Compounds 1 to 6 were tested against 5 human tumor cell lines (human promyelocytic leukemia HL-60, human hepatoma SMMC-7721, human lung adenocarcinoma A-549, human breast cancer cells MCF-7, human colon cancer cell SW-480) did not show cytotoxic activity.