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目的建立了一种能简单准确地测定甲苯磺酸索拉非尼原料药含量的高效液相色谱法(HPLC),并对该方法进行了方法学验证。方法采用HPLC梯度洗脱对甲苯磺酸索拉非尼原料药进行含量测定,色谱柱为Inertsil ODS SP(4.6×150 mm,5μm),流动相A为10 m M磷酸二氢钾缓冲溶液(pH=3.0);流动相B为乙腈—乙醇(1∶1),检测波长为235 nm,柱温为40℃,流速为1.0 ml/min。在实验中通过对系统适用性、精密度、专属性、标准曲线与线性、回收率、重复性等的测定确保方法的准确性。结果索拉非尼与相邻杂质峰之间的分离度良好;索拉非尼在0.02403~0.03605 mg/ml的浓度范围内,线性关系良好;平均回收率为100.20%,RSD为1.05%。结论该方法专属性强,重复性好,准确度高,可用于甲苯磺酸索拉非尼原料药含量的测定。
Objective To establish a high performance liquid chromatography (HPLC) method for the simple and accurate determination of sorafenib tosylate drug substance and verify the method. Methods The content of sorafenib tosylate was eluted by gradient elution. The chromatographic column was Inertsil ODS SP (4.6 × 150 mm, 5 μm). The mobile phase A was 10 mM potassium dihydrogen phosphate buffer solution = 3.0). The mobile phase B was acetonitrile-ethanol (1: 1), the detection wavelength was 235 nm, the column temperature was 40 ℃ and the flow rate was 1.0 ml / min. In the experiment, the accuracy of the method was ensured by the measurement of system suitability, precision, specificity, standard curve and linearity, recovery rate and repeatability. Results Sorafenib had good separation from adjacent impurity peaks. Sorafenib showed a good linearity in the range of 0.02403 ~ 0.03605 mg / ml with an average recovery of 100.20% and a RSD of 1.05%. Conclusion The method is specific, reproducible and accurate. It can be used for the determination of sorafenib tosylate drug substance.