HPLC-ELSD法测定硫酸庆大霉素片的组分和有关物质

Determination of components and related substances in gentamicin sulfate tablets using HPLC-ELSD methods

目的建立硫酸庆大霉素片组分和有关物质测定的HPLC-ELSD法,并采用该方法测定了156批次样品。方法采用ApolloC色谱柱(250mm×4.6mm,5μm),流动相为0.2mol/L三氟乙酸溶液:甲醇(96:4),柱温35℃。ELSD检测:漂移管温度110℃,载气流速2.5L/min,增益1。结果硫酸庆大霉素C组分(C1、C1a、2、C2a)分别在0.0538~0.6729、0.0651~0.8136、0.0299~0.3738和0.0517~0.6465mg/mL浓度范围内线性关系良好,回收率范围为98.1%~101.3%;各辅料与庆大霉素组分和有关物质均能有效分离,不干扰组分和有关物质的测定:8批次样品的庆大霉素总C组分含量偏低,西索米星和总杂含量偏高。结论本方法准确简便,可有效控制硫酸庆大霉素片的组分和有关物质,防止企业采用劣质原料生产片剂。

Objective To establish the HPLC-ELSD method for the determination of components and related substances in gentamicin sulfate tablets,and to determine 156 samples.Methods The column was Apollo C,a(250mm×4.6mm,5μm),mobile phase was 0.2mol/L trifluoroacetic acid solution:methanol(96:4),the column temperature was 35℃,ELSD:drift tube temperature was 110℃,carrier gas flow rate was 2.5L/min,and the gain was 1.Results The linear relationship ranges of C components(C1,C1a,C2,C2a)of gentamicin were 0.0538~0.6729,0.0651~0.8136,0.0299~0.3738 and 0.0517~0.645mg/mL,respectively.The linear relationship in the range was good,and the recovery rate range was 98.1%to 101.3%.The components and related substances of gentamicin could be separated effectively without interfering with the determination of the components and related substances.The contents of total C component of gentamicin in eight samples were low,and the contents of sisomicin and total impurities were high.Conclusion The method is accurate and simple,and can effectively control the components and related substances of gentamicin sulfate tablets,so as to prevent pharmaceutical companies from using inferior raw materials to produce tablets.