摘要
建立了液相色谱-质谱法测定阿哌沙班中的基因毒性杂质3-吗啉基-1-[4-（5-氯戊酰胺基）苯基]-5,6-二氢吡啶-2（1H）-酮（2）。采用Waters Xterra RP18色谱柱,以0.01 mol/L乙酸铵缓冲液∶乙腈为流动相,梯度洗脱。质谱采用电喷雾离子源（ESI）,正离子模式,选择离子监测（SIM）模式,监测离子为m/z 392.2。2在10~100 ng/ml浓度范围内线性关系良好,平均回收率为101.5%,RSD为1.7%。最低检测限和最低定量限为2.015和5.038 ng/ml。
A LC-MS method was established for the determination of the genotoxic impurity, 3-morpholino-1- [4-（5-chloropentamido） phenyl]-5,6-dihydropyridin-2 （1H）-one （2）, in apixaban. A Waters Xterra RP18 column was used, with the mobile phase of 0.01 mol/L ammonium acetate buffer ： acetonitrile by gradient elution. The MS detection was carried out by monitoring m/z 392.2 in selective ion monitoring （SIM） mode with positive electrospray ionization. It was linear for 2 in the range of 10 - 100 ng/ml. The average recovery was 101.5%, with RSD of 1.7%. The LLOD and LLOQ were 2.015 and 5.038 ng/ml, respectively.
出处
《中国医药工业杂志》
CAS
CSCD
北大核心
2015年第9期1004-1007,共4页
Chinese Journal of Pharmaceuticals
