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目的建立高效液相色谱法测定甲苯磺酸索拉非尼起始物料A(SLFN-A)的有关物质的方法,并对其进行方法学验证。方法以Inert Sustain C18(4.6 mm×250 mm,5μm)为色谱柱,20 m M磷酸二氢钾缓冲盐(p H=3.50)为流动相A,甲醇为流动相B,梯度洗脱,流速为1.0 ml/min,柱温为30℃,检测波长为235 nm,进样体积10μl。结果在该条件下,样品中主成分与各杂质之间均能较好分离,在0.15~4.5 mg/ml范围内呈现良好的线性关系(Y=17.891X+0.1954,r=0.9999)。结论该方法法灵敏、准确、专属性好,能对SLFN-A的主要杂质进行有效的分离和检测,可用于该物质的质量控制。
OBJECTIVE To establish a method for the determination of related substances of sorafenib tosylate starting material A (SLFN-A) by high performance liquid chromatography (HPLC) and to verify the method. Methods The mobile phase A was consisted of Inert Sustain C18 (4.6 mm × 250 mm, 5 μm) column, 20 mM potassium dihydrogen phosphate buffer (p H = 3.50), methanol as mobile phase B, gradient elution 1.0 ml / min, the column temperature was 30 ℃, the detection wavelength was 235 nm, the injection volume was 10μl. Results Under this condition, the main components in the sample could be well separated from the impurities, showing a good linear relationship in the range of 0.15-4.5 mg / ml (Y = 17.891X + 0.1954, r = 0.9999). Conclusion The method is sensitive, accurate and specific. It can effectively separate and detect the main impurities of SLFN-A and can be used for the quality control of this substance.