摘要
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 an HPLC method for the determination of related substances in apixaban. Method The self contrast and correction factor method was established to determine the related substances in apixaban simultaneously. Methods validation was also performed. Results The limits of quantitation 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. And the limits of detection for impurities and apixaban were 11.0,22. 0, 17.0,15.0,18.0 and 16.0 μg·L^-1 respectively. There was good linear relationship between response values and contents in the experimental concentration range of five impurities and apixaban （ r ≥0. 999 ）. The recov- ery ranged from 90.0% to 108.0% with RSD ≤4.0%. The content of impurity 1 and unspecified impurity in the sample was 0. 29% and 0. 23‰, and the total impurities was 0. 31%. Conclusions This method can be used to determine the related substances presented in apixaban.
出处
《沈阳药科大学学报》
CAS
CSCD
北大核心
2017年第1期37-42,共6页
Journal of Shenyang Pharmaceutical University
