壮药拟草果中3,5-二羟基-7,4'-二甲氧基黄酮候选化学对照品的制备及其质量控制研究
Preparation and quality control of 3,5-dihydroxy-7,4'-dimethoxyflavone,a candidate reference substance from Zhuang medicine Amomum paratsaoko S.Q.Tong & Y.M.Xia
赖克道 1柴玲 1陈明生 1冯军 1袁健童 1刘布鸣1
作者信息
- 1. 广西壮族自治区中医药研究院广西中药质量标准研究重点实验室,南宁 530022
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摘要
目的:从壮药拟草果中制备纯化3,5-二羟基-7,4'-二甲氧基黄酮候选化学对照品并建立其质量分析方法.方法:采用硅胶柱色谱、重结晶和高效制备液相色谱等,从拟草果中制备纯化得到高纯度的3,5-二羟基-7,4'-二甲氧基黄酮,通过红外、紫外、核磁共振等综合波谱解析方法及质谱确定其化学结构,采用薄层色谱法、高效液相色谱法检测色谱纯度,炽灼残渣法测定灰分,质量平衡法计算3,5-二羟基-7,4'-二甲氧基黄酮的含量.采用高效液相色谱法对建立的3,5-二羟基-7,4'-二甲氧基黄酮候选化学对照品质量分析方法进行方法学考察.结果:3,5-二羟基-7,4'-二甲氧基黄酮候选化学对照品用高效液相色谱法面积归一化法测定的含量均值为99.85％,炽灼残渣法测得灰分值为0.02％,以质量平衡法计算的含量为99.83％.建立的含量测定方法专属性强,精密度良好.结论:制备得到的3,5-二羟基-7,4'-二甲氧基黄酮候选化学对照品符合化学对照品的质量标准要求,可作为拟草果及其他含有此成分的药材与制剂质量控制的对照品.建立的质量分析方法准确、可靠,可为该对照品质量标准研究与制定提供科学依据.
Abstract
Objective:To study the preparation and quality control of 3,5-dihydroxy-7,4'-dimethoxyflavone candidate chemical reference substance from Zhuang medicine Amomum paratsaoko S.Q.Tong & Y.M.Xia.Methods:3,5-dihydroxy-7,4'-dimethoxyflavone was separated and purified consecutively by silica gel,re-crystallization as well as preparative HPLC.The structure of 3,5-dihydroxy-7,4'-dimethoxyflavone was i-dentified by IR,UV,NMR and other comprehensive spectrum analytical methods with MS spectrum.Its purity was determined by HPLC and TLC,the ash content was determined by incandescent residue method,and the con-tent of 3,5-dihydroxy-7,4'-dimethoxyflavone was calculated by mass balance method.The method for qual-ity analysis of 3,5-dihydroxy-7,4'-dimethoxyflavone candidate reference materials was investigated by HPLC.Results:The mean value determined by HPLC of 3,5-dihydroxy-7,4'-dimethoxyflavone was 98.85％,the ash value was 0.02％,and the content of 3,5-dihydroxy-7,4'-dimethoxyflavone calculated by mass balance method was 99.83％.The established analytical method was specific and precise.Conclusion:3,5-Dihydroxy-7,4'-dimethoxyflavone which was prepared in this study met the quality standard require-ments of chemical reference substance,and could be used as a reference substance for quality control of medicinal materials and their preparations such as Amomum paratsaoko S.Q.Tong & Y.M.Xia and others.The analysis method was accurate and reliable,which provided a scientific basis for the research and formulation of quality standard of this reference substance.
关键词
壮药/拟草果/3,5-二羟基-7,4'-二甲氧基黄酮/候选化学对照品/制备纯化/结构鉴定/纯度检查/含量测定Key words
Zhuang medicine/Amomum para-tsaoko S.Q.Tong & Y.M.Xia/3,5-dihydroxy-7,4'-dime-thoxyflavone/candidate chemical reference substance/preparation and purification/structural identification/puri-ty test/content determination引用本文复制引用
基金项目
广西自然科学基金青年基金项目(2017GXNSFBA198091)
广西中药质量标准研究重点实验室自主研究课题(桂中重自201803)
出版年
2024
NETL
NSTL
万方数据