棒柄花叶中胡椒酚-β-D-吡喃葡萄糖苷候选对照品的制备研究

Preparation of candidate reference substance of chavicol-β-D-glucopyranoside from leaves of Cleidion brevipetiolatum

目的:研究胡椒酚-β-D-吡喃葡萄糖苷候选化学对照品的制备方法及其质量标准,为含胡椒酚-β-D-吡喃葡萄糖苷药材及其相关产品的质量控制提供参考。方法:利用硅胶柱色谱和反相制备高效液相色谱对棒柄花叶的乙醇提取物进行分离纯化,分别以薄层色谱法和高效液相色谱法对胡椒酚-β-D-吡喃葡萄糖苷进行纯度检查和含量测定,并通过UV、IR、MS、^(1)H-NMR、^(13)C-NMR等对其进行结构确证。结果:从棒柄花叶中分离、纯化出胡椒酚-β-D-吡喃葡萄糖苷候选对照品C_(15)H_(20)O_(6),其紫外最大吸收波长为273 nm,高分辨质谱结果为HESI-MS m/z 319.11395[M+Na]^(+),薄层色谱检验结果显示供试品为单一斑点,高效液相色谱法纯度测定质量分数W>98.0%。结论:所建立的制备方法简单,制备出的胡椒酚-β-D-吡喃葡萄糖苷对照品符合中药化学对照品的相关要求,可作为棒柄花叶药材和含胡椒酚-β-D-吡喃葡萄糖苷产品质量控制以及中药药效物质基础用的化学对照品。

Objective:To prepare high quality chavicol-β-D-glucopyranoside as candidate reference substance and establish the analysis method for the quality control of medicinal materials and relative products containing chavicol-β-D-glucopyranoside.Methods:Ethanol-extract of the leaves of Cleidion brevipetiolatum was isolated and purified by TLC and HPLC with column chromatography and recrystallization.Its structure was identified by UV,IR,MS,^(1)H-NMR and ^(13)C-NMR.Results:Chavicol-β-D-glucopyranoside C_(15)H_(20)O_6 was completely separated from leaves of Cleidion brevipetiolatum with λ_(max)(CH_(3)OH)at 273 nm by UV and m/z of 319.11395([M+Na]^(+))by HESI-MS.A single spot was detected by TLC and the HPLC purity of the candidate reference substance was above 98.0%.Conclusion:The method is simple and convenient,by which the prepared compound is accorded with the relative standards of chemical reference substance in traditional Chinese medicine.It can be used as a reference substance for the quality control of leaves of Cleidion brevipetiolatum and the research of herbal medicine.