蒽贝素候选化学对照品的制备及分析研究

Preparation and Analysis of Candidate Reference Substance of Embelin

目的研究蒽贝素候选化学对照品的制备方法及其质量标准,为含蒽贝素药材及其相关产品的质量控制提供参考。方法酸藤子用有机溶剂提取,硅胶柱色谱和反相制备型高效液相色谱进行分离纯化、重结晶得到高纯度蒽贝素,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,以质量平衡法计算蒽贝素的含量。结果蒽贝素候选化学对照品高效液相色谱纯度测定均值为99.13%,炽灼残渣测定均值为0.02%,以质量平衡法计算含量为99.11%。结论制备得到的高纯度蒽贝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对照品;建立的分析方法准确、可靠,可为对照品质量控制提供科学依据。

Objective To prepare high quality embelin as candidate reference substance and establish the analysis method for the quality control of medicinal materials and relatvie products containing embelin. Methods Embelin was isolated and purified from diethyl ether-extract of the fruits of Embelia laeta(Linn.)by RP-HPLC combining other column chromatography and recrystallization steps. The structure of embelin was identified by UV,IR,MS and 1H-NMR. The purity was determined by HPLC,the ash content was determined by incandescent residue method,and the content of embelin was calculated by mass balance method. Results The purity calculated based on chromatography was 99.13%,and the ash content was 0.02%. The content of embelin was 99.11% by mass balance method. Conclusion The embelin prepared in this study meets the requirement of chemical reference substance for traditional Chinese medicine and can be used for quality control of herbal medicine and preparation products. The analysis method is accurate and reliable, which provides a scientific basis for quality control of the reference substance.