单磷酸阿糖腺苷有关物质检测方法的优化

Improvement of determination method for related substances in vidarabine monophosphate

目的:优化单磷酸阿糖腺苷有关物质的HPLC测定方法。方法:采用色谱柱ChromCore AQC_(18)(4.6 mm×150 mm, 5μm),流动相A为含0.01 mol·L^(-1)四丁基氢氧化铵与0.1 mol·L^(-1)磷酸二氢钾的缓冲液,流动相B为甲醇,梯度洗脱,流速为1.0 mL·min^(-1),柱温30℃,检测波长258 nm。结果:主成分与各杂质间的分离度良好;主成分及各杂质在各自浓度范围内呈现良好的线性关系(r>0.999 9);单磷酸阿糖腺苷原料药各杂质的平均加样回收率为95.0%~99.2%,RSD为1.0%~4.4%(n=9),注射用单磷酸阿糖腺苷各杂质的平均加样回收率为91.8%~102.1%,RSD为0.5%~4.8%(n=9)。结论:该方法简便、快捷、准确、专属性强,可用于单磷酸阿糖腺苷有关物质的测定。

Objective:To improve the method for the determination of related substances in vidarabine monophosphate.Methods:The analysis was performed on an ChromCore AQC_(18) column(4.6 mm×150 mm,5μm)with mobile phase A of an aqueous solution containing 0.01 mol·L^(-1) tetrabutylammonium hydroxide and 0.1 mol·L^(-1) potassium dihydrogen phosphate and mobile phase B of methanol by gradient elution at the flow rate of 1.0 mL·min^(-1).The column temperature was maintained at 30℃and the UV detection wavelength was set at 258 nm.Results:Related substances were effectively separated from the principal component.Vidarabine monophosphate and its four impurities showed a good linear relationship in the self-concentration ranges(r>0.9999).The average recoveries and were 95.0%-99.2%with RSDs(n=9)of 1.0%-4.4%related substances in vidarabine monophosphate and 91.8%-102.1%with RSDs of 0.5%-4.8%(n=9)for vidarabine monophosphate for injection,respectively.Conclusion:The improved method is simple,rapid and specific,and can be used for the determination of related substances in vidarabine monophosphate.