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胡黄连中酚类化合物的分离及UPLC-ESI-MS分析
刘时乔1, 张新鑫2, 单淇2, 周福军2, 侯文彬1,2
1.天津中医药大学,天津 300193;2.天津药物研究院,天津 300193
摘要:
[目的] 研究胡黄连中的酚性成分,并对其在胡黄连药材中的含量进行测定。[方法] 采用溶剂提取、硅胶柱色谱及葡聚糖凝胶柱色谱等方法分离纯化,根据1H-NMR、13C-NMR和超高效液相色谱与电喷雾质谱(UPLC-ESI-MS)等鉴定化合物的结构,以分离获得的化合物为对照品,采用HPLC-ESI-MS测定其在提取物及药材中的含量。[结果] 从胡黄连中获得6个酚性化合物:云杉苷(Ⅰ)、草夹竹桃苷(Ⅱ)、藏黄连酚苷A(Ⅲ)、藏黄连酚苷F(Ⅳ)、香草酸(Ⅴ)和香草乙酮(Ⅵ).[结论] 上述酚性化合物在胡黄连提取物中的含量分别为1.50%、5.62%、3.53%、1.96%、0.78%和3.16%,在药材中含量分别为0.24%、0.90%、0.56%、0.31%、0.13%、0.51%.
关键词:  胡黄连  UPLC-ESI-MS  酚类化合物  分离
DOI:10.11656/j.issn.1672-1519.2012.06.21
分类号:
基金项目:天津市中药对照品库的建设项目(033187511).
Isolation of phenolic constituents from Picrorhiza scrophulariiflora Pennell and UPLC-ESI-MS analysis
LIU Shi-qiao1, ZHANG Xin-xin2, SHAN Qi2, ZHOU Fu-jun2, HOU Wen-bin1,2
1.Tianjin University of TCM, Tianjin 300193, China;2.Tianjin Institute of Pharmaceutical Research, Tianjin 300193, China
Abstract:
[Objective] To study the Phenolic constituents in Picrorhiza scrophulariiflora Pennell and determine their contents in the medicinal materials. [Methods] The compounds were isolated by the solvent extract, silica gel and Sephadex LH-20 columns and their structure were elucidated by 1H-NMR、13C-NMR and UPLC-ESI-MS which were used as analysis standards. Their contents in the extract and medicinal materials were determined by UPLC-ESI-MS. [Results] Six phenolic compounds were obtained and identified as Picein (Ⅰ), Androsin (Ⅱ), Scrophenoside A(Ⅲ), Scrophenoside F(Ⅳ), Vanillic acid (Ⅴ) and Acetovanillone(Ⅵ). [Conclusion] The contents of above compounds in the extract are 1.50%, 5.62%, 3.53%, 1.96%, 0.78% and 3.16%, and the contents in the medicinal materials are 0.24%, 0.90%, 0.56%, 0.31%, 0.13%, 0.51%, respectively.
Key words:  Picrorhiza scrophulariiflora Pennell  UPLC-ESI-MS  Phenolic constituents  isolation
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