RP-HPLC法测定阿哌沙班片的含量及有关物质

Determination the Content and Related Substances of Apixaban Tablets by RP-HPLC

目的：建立测定阿哌沙班片的含量及有关物质的方法。方法：采用反相高效液相色谱法。色谱柱为Waters XBridge Shield RP18柱,流动相为乙腈-0.05 mol/L磷酸二氢钾溶液（用50%磷酸溶液调节p H至3.0）（20∶80,V/V）,流速为1.0 ml/min,检测波长为293 nm,柱温为25℃,进样量为10μl。结果：在所建立的色谱条件下,阿哌沙班与各杂质及其降解产物分离良好;阿哌沙班的质量浓度在4.30～45.00μg/ml范围内与峰面积积分值呈良好的线性关系（r=0.999 4）;精密度、稳定性、重复性试验的RSD≤1.10%;阿哌沙班的平均加样回收率为99.93%,RSD为0.30%（n=3）;其最大单个杂质的质量分数为0.019%～0.026%,总杂质的质量分数为0.062%～0.074%。结论：本方法操作简便、结果准确、灵敏度高,适用于阿哌沙班片的含量及有关物质测定,对建立阿哌沙班片的质量控制标准有一定的参考价值。

OBJECTIVE： To establish a method for the determination of content and related substances of Apixaban tablets. METHODS ： RP-HPLC was adopted with Water XBridge Shield RP18 column, the mobile phase was acetonitrile -0.05 mol/L potas- sium dihydrogen phosphate solution （adjusted with 50% phosphoric acid to pH 3.0）（20：80, V/V） with flow velocity of 1.0 ml/min. Detection wavelength was set at 293 nm, the column temperature was 25 ℃, the injection volume was 10 μl. RESULTS： Under the establishment of chromatographic conditions, apixaban impurities and its degradation products had a good degree of separation; there was a good linear relationship between the content of apixaban in the range of 4.30 - 45.00 μg/ml and peak area values （r= 0.999 4）. The RSD of precision, stability, repeatability tests were no more than 1.10%, the average recovery of apixaban was 99.93%, RSD was 0.30% （n=3）. The largest single impurity content in mass fraction was in the range of 0.019% to 0.026%, the total impurity content in mass fraction was 0.062% to 0.074%. CONCLUSIONS： The method is simple, accurate, sensitive and can be used to determine the content and related substances of Apixaban tablets. It provides reference for the establishment of the quality control standard of Apixaban tablets.