考察双氢青蒿素(DHA) 差向异构体转化现象对有关物质测定结果的影响,评价并优化2015年版药典中双氢青蒿素有关物质测定方法,采用HPLC-UV法,用十八烷基硅烷键合硅胶(4.6mm×250mm,5μm) 为填充剂,采用梯度洗脱,检测波长为216nm;流速为1.0mL/min,采用甲醇为样品溶剂,且前处理温度不超过25℃.双氢青蒿素进样量在0.193 0～48.25μg(r=1)范围内线性关系良好.α-双氢青蒿素的检出限、定量限分别为0.533 ng、1.78 ng;β-双氢青蒿素的检出限、定量限分别为2.22 ng、7.39 ng.对5批原料药进行有关物质检查,结果均符合药典规定.优化了《中国药典》2015年版中关于双氢青蒿素原料药有关物质检测方法;并弥补了该方法的不足.为双氢青蒿素建立稳定、可靠、全面的质量标准提供科学依据.%In order to investigate the effect of Dihydroartemisinin(DHA) epimer transformation on the determina-tion of related substances, and development and validation for the determination of Dihydroartemisinin’s related sub-stances in ChP 2015, the highperformance liquid chromatography was carried out on a column packed with octade-cylsilane bonded silica gel (4.6 mm×250 mm,5 μm) ,using gradient elution as the mobile phase.The detection wavelength was set at 216 nm and the flow rate was 1.0 mL/min.Methanol was chosen as the solvent for the DHA bulk drug, and the pretreatment temperature not exceeding 25 ℃.Thelinear range of DHA calibration curve was 0.193 0～48.25 μg (r=1).Thedetectionlimitand quantitation limit of α-DHA were 0.533 ng, 1.78 ng, and β-DHA were 2.22 ng、7.39 ng.The five batches of drug substance were examined and the tested results of related substances were all in accordance with the requirements of the pharmacopoeia.Compared with the method include-din ChP,the precision of the established related substances determination method is improved significantly.It is ac-curate,reliable,and comprehensively for evaluation the related substances determination of DHA.
展开▼
