HPLC法测定二对甲苯磺酸缘生替尼原料药中的有关物质  

Determination of Related Substances in Yunsintinib Ditosylate Active Pharmaceutical Ingredients by HPLC

作　　者：仲艳[1] 李家春[1] 李瑛光[1] 王振中[1] 黄文哲[1] 萧伟[1] 

机构地区：[1]江苏康缘药业股份有限公司,江苏连云港222001

出　　处：《中国药房》2017年第3期412-415,共4页China Pharmacy

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 C_(18),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0.25~2.0μg/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。OBJECTIVE： To establish a method for the determination of related substances in yunsintinib ditosylate active phar- maceutical ingredient. METHODS： HPLC was performed on the column of Waters Symmetry C18 with mobile phase of metha- nol-0.01 mol/L ammonium acetate solution （gradient elution）, flow rate was 1.0 mL/min, the detection wavelength was 240 urn, 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, sta- bility 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.

关 键 词：二对甲苯磺酸缘生替尼原料药 高效液相色谱法 有关物质 

分 类 号：R927[医药卫生—药学]