论文部分内容阅读
目的:建立抗癌新药瑞戈非尼中遗传毒性杂质4-(4-氨基-3-氟苯氧基)-N-甲基吡啶-2-甲酰胺(AFP-PMA)的含量测定方法。方法:采用LC-MS/MS法测定;利用Waters XBridge Shield RP_(18)色谱柱(150 mm×3.0 mm,3.5μm)进行分离,以5mmol·L~(-1)乙酸铵溶液(A)-乙腈(B)为流动相,采用梯度洗脱(0~9 min,5%B→90%B),流速为1.0 ml·min~(-1),柱温50℃;ESI离子源,正离子扫描方式,多反应监测(MRM)模式扫描,检测离子通道为m/z 262.2→244.1。结果:AFP-PMA浓度在2.41~980.90 ng·ml~(-1)范围内与峰面积呈良好线性关系(r=0.999 8);定量限为8.02 ng·ml~(-1);检出限为2.41 ng·ml~(-1),约为供试品溶液浓度的0.000 241%;平均加样回收率为100.95%,RSD为2.37%(n=9)。结论:本方法专属性强、灵敏度高、准确度好,可用于瑞戈非尼中4-(4-氨基-3-氟苯氧基)-N-甲基吡啶-2-甲酰胺的含量测定。
OBJECTIVE: To establish a method for the determination of gefitinib-4-amino-3-fluorophenoxy) -N-methylpyridine-2-carboxamide (AFP-PMA) Methods: The compounds were separated by LC-MS / MS and eluted with 5 mmol·L -1 ammonium acetate solution (A) - The mobile phase consisted of acetonitrile (B), gradient elution (0 ~ 9 min, 5% B → 90% B), flow rate 1.0 mL · min -1 and column temperature 50 ℃. Scan mode, multiple reaction monitoring (MRM) mode scan, detection of ion channels m / z 262.2 → 244.1. Results: AFP-PMA showed a good linear relationship with the peak area in the range of 2.41-980.90 ng · ml -1 (r = 0.999 8). The limit of quantification was 8.02 ng · ml -1. The detection limit Was 2.41 ng · ml -1, which was about 0.000 241% of the concentration of the test solution. The average recovery was 100.95% with a RSD of 2.37% (n = 9). Conclusion: The method is specific, sensitive and accurate, and can be used for the determination of 4- (4-amino-3-fluorophenoxy) -N-methylpyridine-2-carboxamide in regarone .