摘要
目的建立高效液相色谱一质谱联用测定甲磺酸伊马替尼中基因毒性杂质伊马胺的方法。方法选用C18色谱柱（3．5μm，150mm×3．0μm），以0．05％甲酸的乙腈-20mmol／L甲酸铵为流动相，采用梯度洗脱进行分离，流速：0．5mL／min；柱温为40％；进样量10μL。对照品溶液选用TSQ Quantum Ultra质谱仪的选择离子检测（SIM）扫描方式进行检测。结果该方法在2．5～100．0ng／ml范围内线性良好（0．998），定量限和检出限分别为2．5ng／mL和1．Ong／mL，方法回收率97．1％，稳定性较好。结论本研究所建立的方法快速、灵敏、专属性强，适用于甲磺酸伊马替尼中基因毒性杂质伊马胺的测定。
Objective A convenient and user-friendly LC-MS/MS analysis method was established for the determination of genotoxic impurity （ N-（5-Amino-2-methylphenyl）-4-（3-pyridyl）-2-pyrimidineamine ） in imatinib mesylale. Methods The method was performed on a Cls （3.5 μL m, 150μm × 3.0μm ）column maintained at 40℃ with a mobile phase of ACN-0.05% methanoic acid and 20mmol/L ammonium formate in a gradient mode; The flow rate was 0.5mL/min and l0 μL L sample solution were injected into the LC-MS/MS system. Detection was carried out by SIM on a TSQ Quantum Ultra LC-MS/MS system. Results The assay was linear over the range 2.5-100.0ng/mL with a limit of quantity-ation of 2.5ng/mL with a limit of detection of 1.0ng/mL. The recovery rate of impurity was 97.1% and the stabilities were good. Conclusion The method is rapid, sensitive, selective, and reliable for the determination of genotoxie impurity （ N-（5-Amino-2-methylphenyl）- 4-（3-pyridyl）-2-pyrimidineamine ） in imatinib mesylate.
出处
《中国医药科学》
2013年第20期36-38,共3页
China Medicine And Pharmacy
关键词
甲磺酸伊马替尼
LC—MS
MS
基因毒性杂质
伊马胺
Imatinib mesylate
LC-MS/MS
Genotoxic impurity
N-（5-Amino-2-methylphenyl）- 4-（3-pyridyl）-2-pyrimidineamine
