水黄皮素候选化学对照品制备及分析研究

Study on the Preparation and Analysis of Candidate Reference Substance of Karanjin

目的:研究水黄皮素候选化学对照品的制备方法及其质量标准,为干花豆药材及其相关产品的质量控制奠定物质基础。方法:采用有机溶剂提取,快速硅胶柱色谱、重结晶和反相制备型高效液相色谱对水黄皮素进行分离纯化,通过波谱等确证化学结构,采用高效液相色谱法测定样品色谱纯度,炽灼残渣法测定灰分,以质量平衡法计算水黄皮素的含量。结果:水黄皮素候选化学对照品高效液相色谱纯度测定均值为98.33%,炽灼残渣测定均值为0.01%;以质量平衡法计算其含量为98.32%。结论:制备得到的高纯度水黄皮素对照品符合中药化学对照品技术要求,可作为中药材或中药复方制剂质量控制的标准品;建立的分析方法准确、可靠,为对照品质量控制提供科学依据。

Objective：To prepare high purity candidate reference substance of Karanjin and establish an analysis method.Methods：Ethanol-extract of the rhizome of Fordia cauliflora Hemsl was isolated and purified by RP-HPLC combining with column chromatography and recrystallization.The structure of Karanjin was identified by UV,IR,MS and 1 HNMR.Its purity was determined by HPLC, the ash content was determined by residue on ignition methodand the content of Karanjin was calculated by mass balance method.Results：The average tested contents of chromatographic purity and ash was 98.33% and 0.01%, respectively.The content of Karanjin was 98.32%by mass balance method.Conclusion：The candidate reference substance of Karanjin can be used for the quality control of herbal medicine.The analysis method is accurate and reliable , and the scientific basis of quality control of the reference substance was provided.