Tongji School of Pharmacy, Huazhong University of Science and Technology, Wuhan 430030, China.
J Pharm Biomed Anal. 2012 Nov;70:26-31. doi: 10.1016/j.jpba.2012.05.010. Epub 2012 May 14.
Imatimib mesylate is a drug for the treatment of gastrointestinal stroma tumor and chronic myelogenous leukemia. In this study, capillary electrophoretic analysis of imatinib mesylate and related compounds was developed. The optimized separation condition was NaH(2)PO(4) (10 mM) aqueous solution containing 5 mM of 2-hydroxypropyl-β-cyclodextrin at a pH of 2.0. The separation could be obtained in less than 20 min when the separation voltage was 20 kV. To enhance the sensitivity, field amplified sample stacking combining with large volume sample injection was adopted. The optimal injection conditions were obtained by using methanol containing 0.5 mM HCl as the sample dilution solution and performing injection at a voltage of 15 kV for 60 s. The linearity ranges of ima amine, N-desmethyl imatinib and imatinib mesylate were 0.005-0.500 μg/ml, and 4-chloromethyl-N-(4-methyl-3-((4-(pyridin-3-yl) pyrimidin-2-yl) amino) phenyl) benzamide was 0.010-0.500 μg/ml, with good linear correlation coefficients (r(2)>0.9900). The intra-day and inter-day relative standard deviations of peak areas were satisfactory. Under the optimized condition, five batches of the synthesized samples were detected and ima amine was found in all the batches. Due to its simplicity, effectiveness and low price, the developed method can be used for quality control analysis of imatinib mesylate.
甲磺酸伊马替尼是一种用于治疗胃肠道间质瘤和慢性髓性白血病的药物。本研究建立了甲磺酸伊马替尼及其相关化合物的毛细管电泳分析方法。优化的分离条件为 pH 2.0 的含 5 mM 2-羟丙基-β-环糊精的 10 mM NaH(2)PO(4)水溶液。当分离电压为 20 kV 时，分离可在不到 20 min 内完成。为了提高灵敏度，采用场放大样品堆积结合大体积进样。通过使用含 0.5 mM HCl 的甲醇作为样品稀释溶液，并在 15 kV 下进样 60 s，获得了最佳的进样条件。伊马胺、N-去甲基伊马替尼和甲磺酸伊马替尼的线性范围分别为 0.005-0.500 μg/ml，4-氯甲基-N-(4-甲基-3-((4-(吡啶-3-基)嘧啶-2-基)氨基)苯基)苯甲酰胺的线性范围为 0.010-0.500 μg/ml，线性相关系数(r(2)>0.9900)良好。峰面积的日内和日间相对标准偏差令人满意。在优化条件下，对五个批次的合成样品进行了检测，发现所有批次均含有伊马胺。由于该方法简单、有效且价格低廉，因此可用于甲磺酸伊马替尼的质量控制分析。
