狗牙根全草的化学成分分离鉴定

目的:研究狗牙根Cynodon dactylon全草的化学成分,丰富狗牙根的化学成分,为狗牙根后续深入研究奠定基础。方法:取狗牙根的干燥全草(20 kg),用95%乙醇加热回流提取3次,合并提取液通过减压浓缩成浸膏。将浸膏用水溶解分散,依次用石油醚,乙酸乙酯,正丁醇3种不同极性的溶剂萃取,减压回收溶剂,得石油醚、乙酸乙酯、正丁醇、水4个不同极性部分的浸膏。采用各种分离技术(包括正向硅胶,反向RP-18,反向小孔树脂(MCI)柱色谱,LH-20羟醛葡聚糖凝胶(sexphadex LH-20),制备薄层色谱和制备HPLC等),对狗牙根乙酸乙酯萃取部位的化学成分进行分离纯化,根据理化性质和波谱分析(1D和2D NMR,UV,MS,CD,ORD)对分离得到的化合物进行结构鉴定。结果:从狗牙根95%乙醇提取物的乙酸乙酯萃取部位中得到8个化合物,分别鉴定为7-oxoarctigenin(1),香草乙酮(2),对羟基苯甲酸(3),(4-hydroxy-3,5-diethoxyphenyl)(3-hydroxy-4-methoxy-phenyl)methanone(4),邻羟基苯甲酸(5),丁香脂素(6),(5S,6S)-5,6-dihydro-3,8,10-trihydroxy-5-(4-hydroxy-3-methoxyphenyl)-6-hydroxymethyl-2,4-dimethoxy-7H-benzoc]xanthen-7-one(7),木犀草素(8)。结论:该研究从狗牙根全草中分离得到的化合物1~8均为首次从该属植物中分离得到。

Chemical Constituents of Whole Plant of Cynodon dactylon

Objective: To separate and identify chemical constituents from Cynodon dactylon which lay a foundation for further research on the effective material of the plant. Method: The dried grass of C.dactylon(20 kg) was extraced with 95% EtOH as the crude extract, and then suspended in water followed by extraction with petroleum ether, EtOAc and nBuOH to acquired four soluble extract successively. The compounds were isolated from the EtOAc extract(150 g) by successive chromatographic procedures(silica gel, RP-18, MCI, Sephadex LH-20, and Semi-preparative HPLC).Their structures were identified by physical and chemical properties and spectral data(1D NMR, 2D NMR, UV, MS, CD, ORD). Result: Eight compounds were separated from C.dactylon and their structures were examined by spectral data and identified as 7-oxoarctigenin(1), together with seven known compounds acetovanillone(2), 4-hydroxybenzoic acid(3), (4-Hydroxy-3, 5-diethoxyphenyl)(3-hydroxy-4-methoxy-phenyl)methanone(4), 2-hydroxybenzoicacid(5), syringaresinol(6), (5S, 6S)-5, 6-dihydro-3, 8, 10-trihydroxy-5-(4-hy-droxy-3-methoxyphenyl)-6-hydrox-ymethyl-2, 4-dimethothoxy-7H-benzoc]xanthen-7-one)(7), and lunteolin(8). Conclusion: Compound 1-8 were isolated from C. dactylon for the first time.