生产过程清洁验证残留物阿哌沙班的HPLC法测定

摘要

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, 5µm)with acetonitrile-water (30∶70) as the mobile phase at the detection wavelength of 280 nm and the lfow velocity of 1.0 ml/min and the column temperature of 30℃ with sample size of 10µl.Results: The standard curve of apixaban showed a good linear relationship in the range of 0.01 to 20µg/ml with the correlation coefifcient (r2) of 0.999 2. The average recovery of samples was 75.90% with RSD of 2.33% (n=18).Conclusion: This method is convenient and accurate and suitable for the quantitative determination of apixaban residues in the cleaning validation.%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 C18（3.9 mm×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，r2=0.9992；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。