【摘要】 目的建立丹参酮ⅡA磺酸钠原料药有关物质检查及含量测定方法。方法采用高效液相色谱法,色谱柱为DiamonsilTMC18(150 mm×4.6 mm,5μm),检测波长为270 nm;流速为1.0 mL.min-1;室温;流动相:以0.1%三乙胺溶液(用磷酸调节pH至4.0)-甲醇(30∶70)为流动相A,以甲醇为流动相B,梯度洗脱,前10 min为流动相A,于5 min内流动相B的比例匀速增加到50%,保持10 min,然后流动相A的比例以20%min-1的比率增加到100%。结果丹参酮ⅡA磺酸钠、丹参酮Ⅰ磺酸和丹参酮检测限分别为0.32、0.32、0.8 ng,丹参酮ⅡA磺酸钠浓度在0.05~0.4 mg.mL-1时,方法线性关系良好(r=0.999 91,n=5),进样精密度RSD为0.65%(n=5)。结论此法简单,结果准确可靠,可用于丹参酮ⅡA磺酸钠原料药的质量控制。更多还原

【Abstract】 OBJECTIVE To determine sulfotanshinone sodium and its relevant substances in bulk drug.METHODSRP-HPLC was adopted.The column was Diamonsil^TMC₁₈（150 mm×4.6 mm,5 μm）,the detection wavelength was 270 nm and the flow rate was 1 mL·min^-1.The chromatography was conducted at room temperature.The system was equilibrated with 100% solution A.Ten minutes after the injection of the solution under test,the proportion of solution B was increased linearly from 0 to 50% at 10% per minute and was maintained at that composition for 10 minutes,after which the proportion of solution A was increased linearly to 100% at 20% per minute.RESULTS The detective limit of sulfotanshinone sodium,sulfotanshinoneⅠsodium and tanshinone Ⅱ_A was 0.32,0.32 and（0.8 ng）,respectively.There was a good linear relationship within（0.05）～(0.4 mg·mL^-1)（（r=）0.999 91,n=5）.The RSD CONCLUSIONS The method proposed for content determination of sulfotanshinone sodium and its relevant substances by HPLC is simple,accurate and can be used in quality control of sulfotanshinone sodium.更多还原