酸浆化学成分及质量控制研究

【作者】 袁野；

【导师】 许枬；

【作者基本信息】 辽宁中医药大学 ， 生药学， 2010， 硕士

【摘要】 目的酸浆宿萼及带果实的宿萼(锦灯笼)为我国传统中药,历代本草均有收载,现代研究表明其酸浆苦素类成分具有较强的抗癌、抗炎等活性,国内外对其化学成分研究颇为关注,但是在我国至今没有完善缺的质量控制标准。因此本文意通过对酸浆宿萼化学成分进行分离、含量测定、指纹图谱、生长因素影响等多方面研究,深入研究酸浆的化学成分组成,分离其对照品,制定药材质量标准,确定其最佳采收期和贮存条件。并且对酸浆全草化学成分开展研究,为扩大酸浆药用资源提供指导。材料和方法材料:茄科植物酸浆(Phyhalis alkekengi L.var.franchetii (Mast.) Makino.)的宿萼及其地上部分。方法:1.采用硅胶、凝胶、氧化铝、ODS柱层析、高效液相等色谱分离技术,利用理化性质和核磁共振光谱、MS等技术,分离鉴定得到的酸浆宿萼及地上部分内主要有效成分。2.采用HPLC法建立酸浆不同采收时间,不同产地,不同药用部位的指纹图谱;测定不同产地,不同采收时间,不同贮存条件下酸浆宿萼酸浆药材的主要有效成分含量变化。结果与结论1.通过对酸浆宿萼进行提取、分离得到含量较大的六个化合物,即酸浆苦素A、酸浆苦素O、酸浆苦素L、酸浆苦素B、酸浆苦素D、木犀草素-7-O-β-D-葡萄糖苷,均可作酸浆药材的质量研究提供了大量对照品。此外还分离得到了11个化合物,经理化常数、波谱解析和化学方法鉴定其中10个化合物,其中二十二烷酸甘油一酯、Cuneataside E、对苯二酚为首次从该植物中分离得到的化合物, 25,27-二脱氢酸浆苦素L为新化合物。2.从酸浆地上部分95%乙醇提取物的乙酸乙酯层分离得到12个化合物,通过理化常数、光谱分析及化学性质鉴定其中8个,分别为商陆素、二十三烷酸、酸浆苦素B、酸浆黄酮醇、酸浆苦素A、酸浆苦素O、酸浆苦素L、酸浆苦素D。地上茎叶部分与宿萼部分主要成分基本相同,差异较小。3.建立20批产地酸浆药材的指纹图谱,并且测定四种酸浆苦素类化学成分含量,制定酸浆药材的质量控制标准。通过指纹图谱和含量测定发现不同产地、不同贮藏时间酸浆药材质量差异明显,初步确定酸浆药材保质期为2年左右。4.首次对酸浆药材的贮藏条件进行研究,发现环境对酸浆药材内酸浆苦素类成分有明显影响,酸浆苦素类成分对温度、紫外线、霉菌均比较敏感,均可以造成酸浆药材质量下降,所以酸浆药材适宜在避光、通风、常温条件下贮藏。并且酸浆采收后不适宜通过机械烘干或阳光下晾晒,应该使其宿萼和果实分离,通风阴干。5.建立不同采收时间酸浆宿萼及地上部分指纹图谱,测定主要有效成分含量变化。通过有效成分动态变化研究确定宿萼的最佳采收期在8月下旬至9月上旬,而酸浆全草与宿萼的采收时间应有所差异。更多还原

【Abstract】 ObjectiveThe calyx seu fructus physalis (jingdenglong) is the traditional chinese herbal medicine, and be documented in all the past Chinese Pharmacopoeia. There is not sutible method to control its quality. So in present thesis we study calyx seu fructus physalis the deals with the isolation, content determinations, chromatographic, Growth factors and so on. To Study the chemical constituents in-deep, to provide quality contral mark, to establish the quality standards, to determine the optimum harvest period and storage conditions.In addition,to expand the resources for meditionl of physalis.,study the chemical constituents of stem and leaves.Material and method:Material:The calyx seu caulis and leaf of phyhalis alkekengi L.var.franchetii (Mast.) Makino. of solanaceae.Method: 1. The chemical constituents of calyx seu and caulis and leaf of phyhalis alkekengi L were isolated by silica gel column chromatography and sephadex LH-20 chromatography technique. On the bases of physic-chemical property and spectroscoie and chemical evidence their structures were identified.2. The chromatographic fingerprint is established by HPLC. The materials are contributed different habitat and harvested in different time and different part of plant were detected. In the mean time, HPLC is carried out to deteminated the content of above materials.Result and Conclusion:1 Big amount of Physalin A, Physalin O, Physalin L, Physalin B, Physalin L, luteolin-7-0-0 -β-D-glucopyranoside were isolated form the caly sue physalis that can provide chemical mark for he quality control. In addition ten of eleven compounds also isolated from the clay sue physalis were identified on the basis of physics and chemistry constant, spectral analysis as well as chemistry method. Including 25,27-dehydro-physalin L were new natural products, and 22 silane acid and Cuneatasid E were isolated from calyx physalis for the first time.2 Twelve compound were isolated from the stems and leaves of phyhalis alkekengi L.seven of them were identified as Tricosanoic Acid, ombuine, Physalin B, physaflavonol, Physalin A, Physalin O, Physalin L, Physalin D.Comparing with clay sue,the main chemical composition is similar,but little difference.3 The fingerprint of the drug of 20 regions of product is established and four physalins were set as the quality standards. The study of fingerprint and content determination indicate that the quantity quality is different significantly among the different habitats and different storage time. We suggest that the valid storage time of clay sue physalis is about 2 years of herbs.4 The storage conditions of physalis alkekengi L was studied for the first time. Result showed that the conditions have significant influence with the contents of physalins. The physalins is sensitive to the temperature, ultraviolet ray and mould.All of them can make the quality of physalis alkekengi L degenerate. So the storage method of clay sue physalis should avoid light and mouldproof at ordinary temperature.In addition, the clay sue physalis should be separated from fruits and placed in the shade and ventilation to dry after harvesting time.5 The chromatographic fingerprint of different harvesting time of sue and stems and leaves of physalis alkekengi L were established and the variations of main effective ingredients were determined. According to the change of contents of the effective ingredients with harvesting time, the optimal harvesting time is late August to early September.更多还原