CAJ | 학술논문

目的：建立高效液相色谱-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×3.0mm），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1.0ng/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。
목적：건립고효액상색보-질보련용측정갑광산이마체니중기인독성잡질이마알적방법。방법선용C18색보주（3.5μm，150mm×3.0mm），이0.05%갑산적을정-20mmol/L갑산안위류동상，채용제도세탈진행분리，류속：0.5mL/min；주온위40℃；진양량10μL。대조품용액선용TSQ Quantum Ultra질보의적선택리자검측（SIM）소묘방식진행검측。결과해방법재2.5～100.0ng/mL범위내선성량호（0.998），정량한화검출한분별위2.5ng/mL화1.0ng/mL，방법회수솔97.1%，은정성교호。결론본연구소건립적방법쾌속、령민、전속성강，괄용우갑광산이마체니중기인독성잡질이마알적측정。
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 mesylate. Methods The method was performed on a C18 (3.5μm,150mm×3.0mm)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 10μL 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 genotoxic impurity(N-(5-Amino-2-methylphenyl)-4-(3-pyridyl)-2-pyrimidineamine)in imatinib mesylate.