注射用去甲斑蝥酸钠中甘露醇的含量测定

Determination of the mannitol as an excipient in sodium demethylcantharidate for injection by HPLC-RID

通过采用磺化交联的苯乙烯二乙烯基苯共聚物为填充剂的强阳离子钙型交换柱,以水为流动相,流速0.5 mL/min,柱温80℃,检测温度为55℃。结果显示:甘露醇在0.04936~0.2468 mg范围内,线性关系良好(r=0.9999),精密度RSD为0.19%,重复性RSD为0.30%,平均回收率为99.34%,RSD为0.67%(n=9)。3个批次的样品含量测定分别为952.5225 mg/g、954.1896 mg/g、345.7485 mg/g。建立高效液相色谱-示差折光检测法(HPLC-RID)测定去甲斑蝥酸钠中辅料甘露醇的含量。此方法专属性强,精密度稳定性良好,准确度较高,可用作注射用斑蝥酸钠中辅料甘露醇的含量测定方法,为完善此药品的检验标准提供参考。

To establish a method for determinating the mannitol as an excipient in sodium demethylcantharidate for injection by HPLC-RID,the test was performed in Carbomix Ca-Np column with water as mobile phase,the flow rate was 0.5 mL/min,the column temperature was 80℃and the detection temperature was 55℃.Results:The linear range falling into 0.04936~0.2468 mg shows good(r=0.9999),the RSD of precision is 0.19%and the RSD of accuracy is 0.30%,the average recovery was 99.34%with RSD as 0.67%(n=9).The contents of mannitol in 3 batches samples was 952.5225 mg/g,954.1896 mg/g,345.7485 mg/g respectively.This estabilished method is reliable,accurate and can be applied for the determination of the mannitol in sodium demethylcantharidate for injection.It provides reference for improving the inspection standard of this drug.