生产过程清洁验证残留物阿哌沙班的HPLC法测定

Determination of apixaban residues in cleaning validation by HPLC

目的:建立清洁验证中残留物阿哌沙班含量测定的高效液相色谱法。方法:色谱柱为Waters Nova-Pak C_(18)(3.9mm×150 mm,5μm),流动相为乙腈-水(30∶70),检测波长280 nm,流速1.0 ml/min,柱温30℃,进样量10μl。结果:阿哌沙班在0.01~20μg/ml范围内线性关系良好,r^2=0.999 2;回收率为75.90%,RSD=2.33%(n=18)。结论:该方法操作简便、结果准确,可以用于清洁验证残留物阿哌沙班的定量分析。

Objective： To establish a method for the determination of apixaban residues in the cleaning validation by HPLC. Methods： HPLC was carried out on a Waters Nova-Pak C18 column （3.9 mm×150 mm, 5 μm） with acetonitrile- water （30 ： 70） as the mobile phase at the detection wavelength of 280 nm and the flow velocity of 1.0 ml/min and the column temperature of 30 ℃ with sample size of 10 μl. Results： The standard curve of apixaban showed a good linear relationship in the range of 0.01 to 20 μg/ml with the correlation coefficient （r2） of 0.999 2. The average recovery of samples was 75.90% with RSD of 2.33% （n=1 8）. Conclusion： This method is convenient and accurate and suitable for the quantitative determination of apixaban residues in the cleaning validation.