抗肿瘤活性化合物SM-1的有关物质检查方法研究

Examination method of related substances of anti-tumor compound SM-1

目的:建立高效液相色谱法检查SM-1的有关物质,为SM-1质量控制提供参考。方法:采用ZORBAX Eclipse XDB-C18柱(250 mm×4.6 mm,5μm)为色谱柱,以0.01 mol·L^(-1)磷酸盐缓冲液[(取0.01mol磷酸氢二钾,加水溶解并稀释至1 000 m L,用磷酸调节p H至(7.0±0.02)]为流动相A,以乙腈为流动相B,梯度洗脱,检测波长210 nm(L2、杂质B及自身对照中的SM-1)和325 nm(SM-1、ABT-D、杂质A及未知杂质)。结果:在上述色谱条件下,SM-1与各副产物及降解产物均能有效分离,杂质L2、ABT-D、杂质A及杂质B的检测限分别为33,15,40,33 ng·m L^(-1)。结论:该方法专属性强、准确、灵敏,可用于SM-1原料药有关物质的检测分析及质量控制。

Objective：To establish an HPLC method for the examination of related substances of SM-1,in order to provide information for the quality control of SM-1. Methods：A ZORBAX Eclipse XDB-C18column（250 mm × 4. 6 mm,5 μm） was used. The mobile phase consisted of solvent A（0. 01 mol·L^-1potassium hydrogen phosphate soulution,p H adjusted to 7. 0 ± 0. 02 by phosphate） and solvent B（acetonitrile）. Gradient elution was adopted. The detection wavelengths were set at 210 nm for related substances L2,B and SM-1 for self-control and325 nm for SM-1,related substances ABT-D,A and unknown related substances,respectively. Results：SM-1 could be separated well with its side products and degradation products. The limits of detection for the related substances L2,ABT-D,A and B were 33,15,40 and 33 ng·m L^-1,respectively. Conclusion：The method is specific,accurate,and sensitive; it can be used for the determination of the related substances of SM-1.