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目的:建立甲磺酸伊马替尼中4-甲基-N-[4-(3-吡啶基)-2-嘧啶基]苯-1,3-二胺的测定方法。方法:采用LC-MS/MS法测定;ESI离子源,正离子模式;用MRM方式进行扫描,选择离子对为278.1/106.1;以甲酸铵溶液-甲酸的乙腈溶液进行梯度洗脱。结果:本成分在1.572~47.160 ng·ml-1范围内线性关系良好(r=0.999 7),检出限为0.002 1 ng,定量限为0.006 8 ng,平均回收率为100.9%(RSD=2.88%),专属性、溶液稳定性、重复性、耐用性等试验结果均符合规定。结论:该法可用于测定甲磺酸伊马替尼中4-甲基-N-[4-(3-吡啶基)-2-嘧啶基]苯-1,3-二胺,明显优于已见报道的其他文献方法。
Objective: To establish a method for the determination of 4-methyl-N- [4- (3-pyridyl) -2-pyrimidinyl] benzene-1,3-diamine in imatinib mesylate. Methods: The LC-MS / MS method was used. The ESI source and positive mode were used. The MRM method was used for scanning. The selected ion pair was 278.1 / 106.1. The gradient elution was carried out with ammonium formate and formic acid in acetonitrile. Results: The linearity was 1.572 ~ 47.160 ng · ml-1 (r = 0.999 7). The detection limit was 0.002 1 ng, the limit of quantification was 0.006 8 ng, and the average recovery was 100.9% (RSD = 2.88 %), Specificity, solution stability, repeatability, durability and other test results are in line with the provisions. Conclusion: This method can be used to determine 4-methyl-N- [4- (3-pyridyl) -2-pyrimidinyl] benzene-1,3-diamine in imatinib mesylate, See other reported literature methods.