董莹 丁金国 黄臻辉

摘 要 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。

关键词 丹参酮ⅡA磺酸钠 有关物质 分离纯化 结构鉴定

中图分类号：R917； R286 文献标志码：A 文章编号：1006-1533（2019）01-0070-04

Isolation and structure identification of sodium tanshinoneⅡA sulfonate

DONG Ying*， DING Jinguo， HUANG Zhenhui**

（Shanghai NO.1 Biochemical and Pharmaceutical Co.， Ltd.， Shanghai 200240， China）

ABSTRACT 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 tanshinoneⅠ sulfonate 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 tanshinoneⅡA sulfonate.

KEy WORDS sodium tanshinone ⅡA sulfonate； relative substances； isolation and purification； structure identification

丹參为唇形科鼠尾草属植物，其根入药，化学成分含脂溶性的二萜醌类和水溶性的酚酸类。丹参酮ⅡA磺酸钠（sodium tanshinoneⅡA sulfonate，STS）是二萜醌类化合物丹参酮ⅡA经磺化而得到的水溶性磺酸盐。临床数据和药理学研究表明，由于其具有抗氧化活性、减少血栓形成、能够降低缺血再灌注所产生的心肌线粒体脂质体过氧化物的含量、改善心肌线粒体膜的流动性、促进旁系血管再生及有效增加冠状动脉流量，对冠心病心绞痛及胸闷、心肌梗死、室性早搏等有显著疗效[1-4]，其注射剂已在临床上广泛使用。

Wang等[5]从STS原料中通过色谱分离纯化、LC- MSn和NMR鉴定推测出8种有关物质；Zou等[6]从STS原料中通过色谱分离纯化、UV、LC-MS和NMR鉴定推测出6种有关物质。而其磺化过程中的副产物和杂质成分研究还不够完善，且该类化合物结构复杂，化学全合成难度大；同时，在STS原料生产和储存过程中均存在产品不稳定的现象，如酸性增强、有效成分降解、含量降低等等。由……