毛菊苣中山柰酚-3-O-β-D-葡萄糖醛酸苷和山柰酚-3-O-β-D-吡喃葡萄糖苷对照品的制备研究  

Preparation of kaempferol-3-O-β-D-glucuronide and kaempferol-3-O-β-D-glucoside reference substances from Cichorium glandulosum

作　　者：肖琴[1] 汪豪[1] 尚靖[2] 叶文才[1,3] 赵守训[1] 

机构地区：[1]中国药科大学天然药物化学教研室,江苏南京210009 [2]中国药科大学新药筛选中心,江苏南京210009 [3]暨南大学中药及天然药物研究所,广东广州510632

出　　处：《西北药学杂志》2011年第3期157-159,共3页Northwest Pharmaceutical Journal

基　　金：国家科技支撑计划项目(编号:2007BAI30B02)

摘　　要：目的建立维药毛菊苣中山柰酚-3-O-β-D-葡萄糖醛酸苷和山柰酚-3-O-β-D-吡喃葡萄糖苷对照品的制备分离方法。方法取毛菊苣药材醇提浸膏的乙酸乙酯萃取部位上样于硅胶柱色谱分离,收集黄酮苷富集流份,继续用凝胶柱色谱及制备HPLC进行分离纯化,通过NMR、MS等波谱方法鉴定化合物结构,经TLC、HPLC-UV及MS联用等技术进行质量分数检测。结果制备分离得到2个化合物分别鉴定为山柰酚-3-O-β-D-葡萄糖醛酸苷(1)和山柰酚-3-O-β-D-吡喃葡萄糖苷(2),质量分数均大于98%,其中2为首次从该属植物中分离得到。结论该法制备得到的2个黄酮苷类对照品符合中药化学对照品的相关技术要求,为药材毛菊苣和含毛菊苣的成方制剂的质量控制及药效物质基础研究提供化学对照品。Objective To establish a simultaneous separation method for reference substances of kaempferol-3-O-β-D-glucuronide and kaempferol-3-O-β-D-glucoside from Cichorium glandulosum.Methods The EtOAc portion from the ethanol extract of C.glandulosum was subjected to column chromatography on silica gel.The collecting fractions was further purified by Sephdex LH-20 column chromatography and preparative HPLC.Their structures were identified by NMR and MS.The purities of the isolates was detected by TLC and HPLC-UV-MS.Results Two compounds were isolated and identified as kaempferol-3-O-β-D-glucuronide（1）and kaempferol-3-O-β-D-glucoside（2）.The TLC and HPLC analysis showed that the purities of the these two compounds were both more than 98%.Compound 2 was isolated from this genus for the first time.Conclusion The two reference substances acquired by this method could meet the demands of the chemical reference substances in Chinese material medica1.It could be used as a reference standard of the quality control and the research of herbal medicine.

关 键 词：毛菊苣 山柰酚-3-O-β-D-葡萄糖醛酸苷 山柰酚-3-O-β-D-吡喃葡萄糖苷 制备高效液相色谱 

分 类 号：R284[医药卫生—中药学]