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目的:建立LC-MS法测定甲磺酸伊马替尼中基因毒性杂质的含量。方法:采用Inertsil ODS-3 C18色谱柱(250 mm×4.6 mm,5μm);流动相A为10 mmol.L-1甲酸铵溶液(用甲酸调pH至3.2),流动相B为甲醇,梯度洗脱(0～10 min,45%B;10～17 min,45%→80%B;17～22 min,80%B;22～23 min,80%→45%B;23～33 min,45%B);流速为1.0 mL.min-1;柱温为35℃;采用正离子模式采集数据。结果:杂质507-00进样是在0.018～0.734 ng范围内,与峰面积呈良好线性关系,线性方程为Y=8.909×104X-453.2,r=0.9999;检测限0.007 ng;定量限为0.018 ng;平均回收率为90.9%,RSD为3.6%(n=9)。结论:本方法简便准确,可用于甲磺酸伊马替尼中基因毒性杂质的检测。
Objective: To establish a LC-MS method for the determination of genotoxic impurities in imatinib mesylate. Methods: The mobile phase A was 10 mmol·L-1 ammonium formate solution (adjusted to pH 3.2 with formic acid) on an Inertsil ODS-3 C18 column (250 mm × 4.6 mm, 5 μm) (0-10 min, 45% B; 10-17 min 45% → 80% B 17-22 min 80% B 22-23 min 80-45% B 23-33 min 45 % B); the flow rate was 1.0 mL.min-1; the column temperature was 35 ℃; the data was collected using the positive ion mode. Results: The impurity 507-00 injection was in the range of 0.018-0.734 ng with a good linear relationship with the peak area. The linear equation was Y = 8.909 × 104X-453.2, r = 0.9999. The detection limit was 0.007 ng. The limit of quantification was 0.018 ng The average recovery was 90.9% with a RSD of 3.6% (n = 9). Conclusion: The method is simple and accurate and can be used to detect genotoxic impurities in imatinib mesylate.