液相色谱-脉冲安培电化学法测定硫酸卡那霉素中各组分含量

建立了一种用反相离子对液相色谱(LC)分离,以金电极为工作电极的脉冲安培电化学法(PAD)直接检测硫酸卡那霉素中主要组分及杂质含量的分析方法。流动相为0.033mol/L草酸、0.012mol/L七氟丁酸、105mL/L乙腈,用稀NaOH调节pH至3.4。考察了各色谱参数对分离测定的影响。实验证明,本方法不需要衍生化,可直接检测硫酸卡那霉素。与报道的其它方法相比,本方法不仅能使硫酸卡那霉素中的卡那霉素A、B得到了很好的分离,还分离出了其它一些未能确证的组分。如用质谱法等对未知组分进行确证后,对硫酸卡那霉素原料药、注射液、滴眼液及兽药等实际样品中的卡那霉素各组分进行测定。可望成为一种标准分析方法。

Determination of Kanamycin Sulfate by Liquid Chromatography with Pulsed Amperometric Detection

A liquid chromatography(LC)with pulsed amperometric detection(PAD)method for the determination of kanamycin on a gold electode was developed.The mobile phase consisted of an aqueous solution containing 0.033 mol/L oxalic acid,0.012 mol/L heptafluorobutyric acid and 105 mL/L acetonitrile with pH 3.40 adjusting by dilute NaOH solution.In comparison with the methods previously published,the total analysis time was short not more than 35 min,and the method allows not only a better separation of kanamycin A and kanamycin B,but also the separation of several other minor components,although most of which were not identified.The effects of the different chromatographic parameters on the separation were also investigated.The method was simple,accurate and wihtout requirement for derivatization steps.