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目的建立高效液相色谱法定量测定阿哌沙班中有关物质。方法采用加校正因子的主成分自身对照法,对阿哌沙班中有关物质进行定量分析,并对该方法进行了方法学验证。结果杂质1、杂质2、杂质3、杂质4、杂质5及阿哌沙班的定量限分别为38.0、75.0、57.0、49.0、58.0和52.0μg·L~(-1);检测限分别为11.0、22.0、17.0、15.0、18.0和16.0μg·L~(-1)。各杂质的线性关系良好(r≥0.999),样品低、中、高三个水平的回收率均在90.0%~108.0%内,RSD≤4.0%。样品中杂质1含量质量分数为0.29%,最大未知单杂质含量质量分数为0.23‰,总杂质含量质量分数为0.31%。结论该方法可用于测定阿哌沙班中有关物质。
Objective To establish a HPLC method for the quantitative determination of apixaban in related substances. Methods The principal component self-control method with correction factor was used to quantitatively analyze the related substances in apixaban, and the method was verified by methodology. Results The limit of quantification for impurity 1, impurity 2, impurity 3, impurity 4, impurity 5 and apixaban were 38.0, 75.0, 57.0, 49.0, 58.0 and 52.0 μg · L -1, respectively. The detection limits were 11.0 , 22.0, 17.0, 15.0, 18.0 and 16.0 μg · L -1, respectively. The linearity of the impurities was good (r≥0.999). The recoveries of the samples at the low, medium and high levels were within 90.0% ~ 108.0% with RSD≤4.0%. The content of impurity 1 in the sample is 0.29%, the content of the largest unknown single impurity is 0.23 ‰, and the total impurity content is 0.31%. Conclusion This method can be used to determine the related substances in apixaban.