HPLC法考察硫酸奈替米星注射液中依地酸二钠的含量

Determination of disodium edetate in Netilmicin Sulfate Injection by HPLC

目的采用高效液相色谱法考察硫酸奈替米星注射液中依地酸二钠的含量。方法以Agilent Zorbax-C_(18)(4.6 mm×250 mm,5μm)为色谱柱;以(四丁基氯化铵2.4 g+醋酸钠4 g+990 mL水溶解,冰醋酸调pH至4.0,加水稀释至1 L)为A相,B相为乙腈-A相(6∶4),流速为1.0 mL·min^(-1),检测波长为350 nm。结果依地酸二钠线性范围为15~62.5μg·mL^(-1),相关系数为0.999 9;平均回收率为102.5%,RSD为1.19%(n=6)。16批次硫酸奈替米星注射液中的依地酸二钠含量均符合规定。本方法与滴定方法测得3批依地酸二钠原料含量无显著差异。结论该方法专属性强,重复性好,适用于硫酸奈替米星注射液中依地酸二钠的质量控制。

Objective To establish HPLC method for the determination of disodium edetate in Netilmicin Sulfate Injection.Methods The chromatographic separation was performed on Agilent ZORBAX-C18（4.6 mm×250 mm,5 μm）.The mobile phase was an aqueous solution comprising 0.24%（M/V） tetrabutylammonium chloride and 0.4%（M/V） sodium acetate（pH was adjusted to 4.0 with acetic acid）.The flow rate was 1.0 mL·min^-1.The detection was carried out at 350 nm.Results The linear range was 15 ～ 62.5 μg·mL^-1 and the correlation coefficient was 0.999 9.The average recovery was102.5% with RSD of 1.19%（n = 6）. The disodium edetate＇ s contents in Netilmicin Sulfate Injection of 16 batches are all accorded with the regulation.There was no significant difference between the results of HPLC and titration analysis method on the same three batches EDTA.Conclusion The method was simple and specific,accuracy and reproducible for controlling the content of disodium edetate in Netilmicin Sulfate Injection.