复方丹参滴丸国际申报项目自制对照品的制备研究

Study on preparation of self-made reference substance for international application project of compound salvia miltiorrhiza dropping pills

目的:制备满足复方丹参滴丸申报FDA过程中产品质量研究及检测所需的对照品。方法:采用柱层析法从三七中提取分离并纯化得到3个单体化合物三七皂苷R_(1)、人参皂苷Rg_(1)和人参皂苷Re,采用紫外、红外光谱、质谱、核磁对其进行结构鉴定,以质量守恒法计算相对纯度,分装得到自制对照品,并对其进行长期稳定性考查。结果:制备得到三七皂苷R_(1)、人参皂苷Rg_(1)和人参皂苷Re,相对纯度分别为94.39%、97.39%和95.00%,长期稳定性研究表明所有对照品24个月稳定性良好,未见降解。结论:通过提取纯化得到3个自制对照品候选物,并通过均一化、结构鉴定、纯度定值,分装成为对照品,满足FDA申报需求。

Objective:To prepare a reference substance for quality study and detection of compound salvia miltiorrhizae dropping pills in the process of FDA application.Methods:Three monomer compounds,notoginsenoside R_(1),ginsenoside Rg_(1),and ginsenoside Re,were isolated and purified from Panax notoginseng by column chromatography.These structures were identified by UV,IR,MS,NMR spectra,and the relative purity was calculated by the mass conservation method.The self-made reference substance was obtained by packing,and the long-term stability was tested.Results:Panax notoginsenoside R_(1),ginsenoside Rg_(1),and ginsenoside Re were prepared with relative purity of 94.39%,97.39%,and 95.00%,respectively.The long-term stability study showed that all the reference substances had good stability after 24 months without degradation.Conclusion:Three self-made reference substances candidates were obtained through identification,value determination,and stability study,meeting the requirements of FDA application.