Sodium Tanshinone IIA Sulfonate, the chemical modification product of Tanshinon IIA (STIIAS) is widely used in clinical treatment of angiocardiopathy, and the preparation of reference compounds of related substances for quality control is necessary. A method for separating three related substances from the bulk drug of STIIAS with high-speed counter-current chromatography (HSCCC) was developed. A solvent system composed of chloroform–n-butanol–methanol–water (17:0.3:14:9) was used and 0.5% saturated ammonium acetate aqueous solution was added to depress the emulsification in order to enhance sample loading capacity. Twelve related substances were identified in the bulk drug by HPLC-DAD and liquid chromatography/multistage tandem mass spectrometry (LC–MSⁿ). Among them, three compounds were prepared and confirmed with ¹H NMR, one was identified without pretreatment, and seven components were identified after HSCCC enrichment since the contents of them were too low to be detected through direct LC–MSⁿ injection. This research successfully broadened the application of HSCCC and introduced it to the field of impurities preparation of chemical medicine.

丹参酮IIA（STIIAS）的化学修饰产品-丹参酮IIA磺酸钠被广泛用于血管性心脏病的临床治疗，因此有必要制备相关物质的参考化合物以进行质量控制。提出了一种利用高速逆流色谱法从STIIAS原料药中分离出三种相关物质的方法。使用由氯仿-正丁醇-甲醇-水（17：0.3：14：9）组成的溶剂系统，并添加0.5％饱和乙酸铵水溶液以抑制乳化，以增强样品的负载能力。HPLC-DAD和液相色谱/多级串联质谱法（LC–MS ⁿ）。其中，制备了三种化合物，并通过¹ H NMR进行了确认，一种未经预处理而被鉴定，并且在HSCCC富集后鉴定出了七种成分，因为它们的含量太低而无法通过直接LC-MS ⁿ进样检测到。该研究成功地拓宽了HSCCC的应用范围，并将其引入化学药物杂质制备领域。