目的:建立并优化二丁酰环磷腺苷钠有关物质检测方法。方法:在日本药局方基础上，对各实验条件进行优化，得到最优检测条件，色谱柱为CAPCELL PAK C18，流动相为pH 6。0磷酸盐缓冲液-甲醇，梯度洗脱，检测波长为258 nm，并进行了方法学验证。结果:系统适用性溶液中，各破坏溶液中主峰与相邻峰之间的分离度均大于1。5;溶液在48 h内稳定;各杂质含量在其限度浓度的50％～150％范围内与峰面积均呈现良好的线性关系，R2＞0。999 4;加标实验中，N6-丁酰3'，5-环磷腺苷钠平均回收率为99。4％～106。6％;2'-O-丁酰3'，5-环磷腺苷钠平均回收率为88。8％～103。6％，环磷腺苷钠平均回收率96。9％～102。5％，均符合要求，对3批样品进行检测，均检出上述杂质。结论:该方法灵敏度高，分离效果、准确性、耐用性好，可用于二丁酰环磷腺苷钠有关物质检测，为其质量控制提供依据。
Optimization and evaluation of detection method for related substances in bucladesine sodium
Objective:To establish and optimize a detection method of dibutyryl cyclic adenosine phosphate related substances.Methods:On the basis of the JP,the experimental conditions were optimized to obtain the optimal detection conditions.The column was CAPCEILPAK C18;mobile phase was pH 6.0 phosphate buffer solution-meth-anol with gradient elution;detection wavelength was 258 mm.The method validation was carried out.Results:In the system applicability solution,the separation degree of the main peak and adjacent peaks in each destruction solution was greater than 1.5;the solution was stable within 48 h.The content of each impurity showed a good line-ar relationship with the peak area in the range of 50％-150％of the limit concentration,R2＞0.999 4.In the spike experiment,the average recovery rate of N6-butyryl 3',5-cyclophosphatin sodium was 99.4％-106.6％.The average recoveries of 2'-0 butyryl 3,5-cycloadenosine monophosphate sodium were 88.8％-103.6％,and the average recoveries of cyclophosphaminate sodium were 96.9％-102.5％,which met the requirements.Three bat-ches of samples were tested,and the above impurities were detected.Conclusion:This method has high sensitivi-ty,good separation effect,accuracy and durability,and can be used for the detection of bucladesine sodium,provi-ding a basis for its quality control.
万方数据
维普
