论文部分内容阅读
目的建立高效液相色谱梯度法测定氟康唑原料药的有关物质。方法采用十八烷基硅烷键合硅胶为填充剂,流动相A为0.01 mol.L-1甲酸铵,流动相B为乙腈,梯度洗脱,流速为0.5 mL.min-1,检测波长为261 nm,进样量为20μL。结果降解产物和杂质在该色谱条件分离良好,氟康唑与杂质B～D在2.632～21.06、2.688～53.76、0.853 6～21.34、2.595～20.76μg.mL-1之间线性关系良好,检测限分别为0.20、0.005 2、0.007 3、0.13μg.mL-1,对来自9个厂家17批氟康唑原料药(含国外5批)进行了测定,各杂质能有效检出。结论该方法简便、快速、灵敏、准确,可用于测定氟康唑原料药的有关物质。
Objective To establish a high performance liquid chromatography gradient method for the determination of related substances of fluconazole. Methods The octadecylsilane bonded silica gel was used as the filler. The mobile phase A was 0.01 mol·L-1 ammonium formate and the mobile phase B was acetonitrile. The gradient elution was performed with a flow rate of 0.5 mL · min-1. The detection wavelength was 261 nm, injection volume of 20μL. Results The degradation products and impurities were separated well under the chromatographic conditions. Fluconazole showed a good linear relationship with impurity B ~ D at the ranges of 2.632 ~ 21.06, 2.688 ~ 53.76, 0.853 6 ~ 21.34, 2.595 ~ 20.76μg.mL-1, Respectively 0.20,0.005 2,0.007 3,0.13μg.mL-1, 17 batches of raw materials from nine manufacturers of fluconazole (including 5 batches abroad) were determined, the impurities can be detected effectively. Conclusion The method is simple, rapid, sensitive and accurate and can be used to determine the related substances of fluconazole.