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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Ion PacAS11-HC(4mm×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 m L·min-1,进样量10μL,以带DIONEX AERS5004-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·m L-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 method for the determination of cytidine triphosphate disodium injection and the determination of related substances by ion chromatography. Methods: Ion PacAS11-HC (4 mm × 250 mm) column was used with potassium hydroxide as the eluent and gradient elution at a flow rate of 1.0 mL · min-1. The injection volume was 10 μL, AERS5004-mm suppressor conductance detector for detection, content of cytidine disodium phosphate injection according to the peak area outside the standard method of calculation, the main degradation of impurities (disodium diphosphate, monosodium cytidine disodium) Calculated according to the principal component self-control method with correction factor. Results: The linearity of sodium cytidine triphosphate was good (r = 0.999 8, n = 6) in the range of 0.000 164-1.60 mg · m L-1. The average recovery was 100.1% The stability of the SDP reference solution was good within 24 h (RSD = 1.3%); CTP-Na2 and CDP-Na2, the main degradation impurity, The limit of quantification (CMP-Na2) was 1.6, 4.57 and 6.0 ng, and the detection limits were 0.50, 1.48 and 1.88 ng, respectively. Conclusion: The method is suitable for the quality control of disodium cytidine triphosphate injection.