基于HPLC特征图谱与制备分离技术川木通标准汤剂化学成分研究

Study on Chemical Constituents of Caulis Clematidis Armandii Standard Decoction Based on HPLC Specific Chromatogram and Preparation Separation Techniques

目的:建立川木通标准汤剂特征图谱,结合柱色谱和制备色谱分离技术对未知特征峰进行分离、纯化和结构鉴定,为川木通标准汤剂及其制剂质量标准的提高提供参考。方法:制备12批川木通标准汤剂,采用高效液相色谱法(HPLC)建立川木通标准汤剂特征图谱,将十八烷基硅烷键合硅胶填料(ODS)的柱色谱和半制备高效液相色谱相结合,对川木通标准汤剂特征图谱的特征峰进行分离、纯化,并采用核磁共振(NMR)和质谱(MS)分析对分离得到的未知化合物进行结构鉴定。结果:12批川木通标准汤剂特征图谱共标识出7个共有特征峰,其整体相似度均在0.90以上。经分离制备和结构分析,共鉴定出5个化合物,分别为腺苷、落叶松树脂醇-4,4′-二-O-β-D-吡喃葡萄糖苷、落叶松树脂醇-4-O-β-D-吡喃葡萄糖苷、开环异落叶松树脂酚和落叶松树脂醇,其中腺苷、开环异落叶松树脂酚和落叶松树脂醇系首次从川木通中分离得到。结论:通过对川木通中极性较大的水溶性成分的研究,为川木通药材、饮片及其制剂质量标准的提高提供有益参考。

Objective:To provide reference for improving the quality standards of Caulis Clematidis Armandii standard decoction and its preparations,the specific chromatogram of Caulis Clematidis Armandii standard decoction was established and the unknown characteristic peaks were separated,purified,and identified by column chromatography and preparative chromatography separation techniques.Methods:12 batches of Caulis Clematidis Armandii standard decoction were prepared,and the specific chromatograms of Caulis Clematidis Armandii standard decoction were established using high-performance liquid chromatography(HPLC).The column chromatography of octadecylsilane bonded silica(ODS)gel packing and semi preparative high-performance liquid chromatography were combined to separate and purify the characteristic peaks of Caulis Clematidis Armandii standard decoction.The structure of the isolated unknown compounds was identified using nuclear magnetic resonance(NMR)and mass spectrometry(MS)analysis.Results:A total of 7 common characteristic peaks were identified in the specific chromatograms of 12 batches of Caulis Clematidis Armandii standard decoction,with an overall similarity of over 0.90.After separation,preparation,and structural analysis,a total of 5 compounds were identified,namely adenosine,lariciresinol-4,4′-bis-O-β-D-glucopyranoside,lariciresinol-4-O-β-D-glucopyranoside,secoisolariciresinol and lariciresinol.Among them,adenosine,secoisolariciresinol and lariciresinol were first isolated from Caulis Clematidis Armandii.Conclusion:This study provides useful references for improving the quality standards of Caulis Clematidis Armandii medicinal materials,decoction pieces,and preparations by studying the highly polar water-soluble components in Caulis Clematidis Armandii.