注射用三磷酸胞苷二钠有关物质检验方法的建立

目的:建立注射用三磷酸胞苷二钠(CTP-Na2)有关物质检验方法。方法:采用高效液相色谱法,以C18为填充柱,以含反相离子对试剂的磷酸盐缓冲液为流动相0.02 mol·L^-1磷酸盐缓冲液-乙腈(90∶10)];流速:1.0 mL·min^-1;检测波长:271 nm;柱温:35℃,采用校正因子计算有关物质。结果:CTP-Na 2在0.093~1.860 mg·mL^-1范围内,溶液的浓度与峰面积的线性关系良好,r=0.9997;平均回收率为99.6%(RSD=1.5%,n=9),CTP-Na2对照品溶液在25 h内的稳定性良好(RSD=0.7%);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4.1、2.1、2.8 ng,检出限分别为0.82、0.16、0.22 ng。结论:现行质量标准中有关物质项存在诸多问题,新建的检测方法操作简便、灵敏度高,可用于质量控制。

Establishment of a method for the determination of related substances in cytidine disodium triphosphate for injection

Objective:To establish a method for determination of related substances in cytidine disodium triphosphate(CTP-Na2)for injection.Methods:The test was performed in C18 column under the elution of phosphate buffer with reverse phase ion-pair reagent(0.02 mol·L^-1 phosphate buffer-acetonitrile(90∶10)).The flow rate was 1.0 mL·min^-1,the detection wavelength was 271 nm,and the column temperature was set at 35℃.The related substanceswas calculated by correction factor.Results:The linear range of cytidine disodium triphosphate fell into 0.0931.860 mg·mL-1(r=0.9997).The average recovery was 99.6%(RSD=1.5%,n=9).The solution of CTP-Na 2 reference substance was stable within 25 hours(RSD=0.7%).The limits of quantitation of CTP-Na2 and the main degradation impurities CDP-Na2,CMP-Na2 were 4.1,2.1,2.8 ng respectively;the limits of detection of them were 0.82,0.16,0.22 ng respectively.Conclusion:There are many problems in the related substances in the current specification.The newly established method is simple and sensitive,and it can be used for quality control.