离子色谱-抑制电导检测法测定环磷酰胺相关物质A的含量

Determination of Cyclophosphamide Related Substance A by Ion Chromatography-Suppressed Conductivity Detection

摘要: 目的采用离子色谱-抑制电导检测法测定环磷酰胺相关物质A的含量。方法采用色谱柱lonPac CS12A (250 mm×4.0 mm Analytical)，以0.16%甲烷磺酸为流动相，流速为1.0 mL·min^-1，检测器为电导检测器，柱温为25 ℃，进样量为25 μL。结果环磷酰胺相关物质A的定量下限为1.8 μg·mL^-1，检测限为0.54 μg·mL^-1；在1.8~24 μg·mL^-1内线性关系良好(r>0.999)，在不同浓度水平范围内的平均回收率为97.45%~99.81%，RSD<3%。结论本方法选择性好，灵敏度高，结果可靠，可满足环磷酰胺相关物质A检验分析的需要。

Abstract: OBJECTIVE To establish ion exchange chromatography-suppressed conductivity detection for the determination of related substance A in cyclophosphamide. METHODS Using a Ionpac CS12A column (250 mm×4.0 mm Analytical), the mobile phase was 0.16% methane sulfonic acid, the flow rate was 1.0 mL·min^-1 with suppressed conductivity detector; the column temperature was 25 ℃; and the inject volume was 25 μL. RESULTS The detection and quantification limit was 0.54 and 1.8 μg·mL^-1, respectively. The linear range for the content of degradation impurity A was 1.8-24 μg·mL^-1(r>0.999), the average recoveries were in the range of 97.45%-99.81% with the relative standard deviation below 3%. CONCLUSION The method is simple, rapid, accurate and is suitable for the determination of cyclophosphamide degradation impurity A.