离子色谱法检测三磷酸胞苷二钠注射液含量及有关物质

目的: 建立用于三磷酸胞苷二钠注射液含量测定及有关物质检测的离子色谱方法。方法: 采用IonPac^®AS11-HC(4 mm×250 mm)色谱柱,以氢氧化钾为淋洗液,采用梯度洗脱,流速为1.0 mL · min^-1,进样量10 μL,以带DIONEX AERS^®500 4-mm抑制器的电导检测器进行检测,三磷酸胞苷二钠注射液的含量按峰面积以外标法计算,主要降解杂质(二磷酸胞苷二钠、单磷酸胞苷二钠)按加校正因子的主成分自身对照法计算。结果: 三磷酸胞苷二钠在0.000 164~1.60 mg · mL^-1 范围内线性关系良好(r=0.999 8,n=6);平均加样回收率(n=9)为100.1%;三磷酸胞苷二钠对照品溶液在24 h内的稳定性良好(RSD=1.3%);三磷酸胞苷二钠(CTP-Na₂)及主要降解杂质二磷酸胞苷二钠(CDP-Na₂)、单磷酸胞苷二钠(CMP-Na₂)的方法定量限分别为1.6、4.57、6.0 ng,检出限分别为0.50、1.48、1.88 ng。结论: 本方法适用于三磷酸胞苷二钠注射液的质量控制。

Objective: To establish a new method for determination and assay of cytidine disodium triphosphate(CTP-Na₂)injection and related substances by ion chromatography. Methods: The IonPac^®AS11-HC column(4 mm×250 mm)was adopted with KOH solution of gradient elution at the flow rate of 1.0 mL · min^-1.The injection volume was 10 μL, and the substances were detected conductively with the DIONEX AERS^®500 4-mm suppressor.The content computation was performed with the peak area external reference method.The main degradation impurities(cytidine disodium diphosphate(CDP-Na₂)and cytidine disodium monophosphate(CMP-Na₂))were determined with the correction factor comparison method to calculate principal components. Results: The linear range of cytidine disodium triphosphate was 0.000 164-1.60 mg · mL^-1 (r=0.999 8, n=6).The average recovery(n=9)was 100.1%.The solution of CTP-Na₂ reference substance was stable within 24 hours(RSD=1.3%), the limits of quantitation of CTP-Na₂ and the main degradation impurities CDP-Na₂, CMP-Na₂ were 1.6 ng, 4.57 ng, 6.0 ng;the limits of detection were 0.50 ng, 1.48 ng, 1.88 ng. Conclusion: The developed method can be applied to quality control of cytidine disodium triphosphate.