HPLC自身校正因子法测定吡嗪酰胺片有关物质

Determination of Related Substances in Pyrazinamide Tablets by HPLC Self-correction Factor Method

目的:建立高效液相色谱(HPLC)法测定吡嗪酰胺片有关物质。方法:色谱柱:Ultimate Polar-RP,4.6*150 mm,5μm;柱温30℃,检测波长为268 nm;流动相:pH 3.0缓冲盐溶液-乙腈-四氢呋喃=1000∶10∶1,用校正因子自身对照法。结果:吡嗪酰胺与杂质A与杂质B分离度均大于1.5,呈良好线性关系,杂质A回收率为100.5%~102.0%,杂质B回收率101.3%~103.1%,精密度良好,重复性良好,在酸、碱、氧化、光、热和湿等条件下的各强制降解实验中,空白样品在主峰及各杂质保留时间处没有显著干扰,稳定性好。结论:该方法灵敏,专属性好,稳定可控,可用于吡嗪酰胺片有关物质的分析研究。

Objective:To establish a high performance liquid chromatography(HPLC)method was established for the determination of related substances in pyrazinamide tablets.Method:Chromatographic column:Ultimate Polar-RP,4.6*150 mm,5μm;The column temperature is 30℃and the detection wavelength is 268 nm;Mobile phase:pH 3.0 buffer salt solution-acetonitrile-tetrahydrofuran=1000∶10∶1,using the correction factor self-control method.Results:The resolution of pyrazinamide and impurity A and impurity B is greater than 1.5,showing a good linear relationship.The recovery rate of impurity A is 100.5%~102.0%,and the recovery rate of impurity B is 101.3%~103.1%.The precision is good and the repeatability is good.In the forced degradation tests under acid,alkali,oxidation,light,heat and humidity conditions,the blank sample has no significant interference at the main peak and the retention time of each impurity,and has good stability.Conclusion:The method is sensitive,specific,stable and controllable,and can be used for the analysis of pyrazinamide tablets.