【摘要】 目的:建立测定二对甲苯磺酸缘生替尼原料药中有关物质的方法。方法:采用高效液相色谱法。色谱柱为Waters Symmetry C₁₈,流动相为甲醇-0.01 mol/L乙酸铵溶液（梯度洗脱）,流速为1.0 mL/min,检测波长为240 nm,柱温为40℃,进样量为10μL。结果:在该色谱条件下,主成分峰与各杂质峰分离度均良好;杂质A、B、C和二对甲苯磺酸缘生替尼检测质量浓度线性范围均为0.25².0μg/mL（r≥0.999 0）,杂质A、B、C的定量限分别为0.5、0.5、2.5 ng;精密度、稳定性、重复性试验的RSD<1.0%;加样回收率分别为97.9%¹02.6%、95.1%¹07.7%、95.8%¹07.5%,RSD分别为1.4%、4.2%、4.1%（n=9）。结论:该方法专属性好、操作简便,可用于二对甲苯磺酸缘生替尼原料药中有关物质的测定。更多还原

【Abstract】 OBJECTIVE:To establish a method for the determination of related substances in yunsintinib ditosylate active pharmaceutical ingredient. METHODS:HPLC was performed on the column of Waters Symmetry C₁₈ with mobile phase of methanol-0.01 mol/L ammonium acetate solution（gradient elution）,flow rate was 1.0 mL/min,the detection wavelength was 240 nm,column temperature was 40 ℃,and injection volume was 10 μL. RESULTS:Under the chromatographic conditions,the main peaks and each impurity peak were well separated;The linear range of impurity A,B,C and yunsintinib ditosylaie were 0.25-2.0 μg/mL（r≥0.999 0）;the quantification limits of impurity A,B and C were 0.5,0.5 and 2.5 ng,respectively;RSDs of precision,stability and reproducibility tests were lower than 1.0%;recoveries were 97.9%- 102.6%（RSD=1.4%,n=9）,95.1%- 107.7%（RSD=4.2%,n=9）,95.8%-107.5%（RSD=4.1%,n=9）,respectively. CONCLUSIONS:The method is specific and simple,and can be used for the determination of related substances in yunsintinib ditosylate active pharmaceutical ingredients.更多还原