丹参酮ⅡA磺酸钠有关物质纯化与结构鉴定

Isolation and structure identification of sodium tanshinone ⅡA sulfonate

目的 :对丹参酮ⅡA磺酸钠原料生产工艺中的主要有关物质进行纯化和结构鉴定。方法 :采用制备高效液相色谱法,对其有关物质进行富集和分离纯化,最终获得HPLC纯度>98%的目标组分。冷冻干燥后,分别进行MS和NMR分析及结构鉴定和解析。结果与结论 :鉴定得到三种有关物质,结构确证为丹参酮ⅡB磺酸钠、丹参酮Ⅰ磺酸钠、紫丹参甲素磺酸钠。这为丹参酮ⅡA磺酸钠原料药及制剂的质量控制、标准提高和稳定性研究提供对照品及依据。

Objective:The purification and structure identification of the related substances remained in production process of the raw material of sodium tanshinoneⅡA sulfonate were performed.Methods:The related substances with HPLC purity over 98%were obtained by preparative HPLC after they were enriched,isolated and purified.After freeze-drying process,these substances were analyzed by MS and NMR and their structures were identified and elucidated.Results&Conclusion:Three related substances were obtained and confirmed as sodium tanshinoneⅡB sulfonate,sodium tanshinoneⅠsulfonate and sodium przewaquinone sulfonate,respectively,which were provided reference samples and scientific basis for the quality control,standard improvement and stability study of the raw material and preparations of sodium tanshinoneⅡAsulfonate.