Abstract: Secondary derivative differential pulse polarography was developedand used for the quantitative analysis of ribostamycin sulfate, kanamycin and their prepa-rations. By using sodium hydroxide-potassium dihydrogen phosphate solution as thebase solution, ribostamycin sulfate and kanamycin showed good peaks at 0.105 V and- 0.37 V (vs Ag/AgCl) respectively. The linear relationship of ribostamycin sulfate andkanamycin between concentration and peak height was obtained in the concentrationrange of 1.8 ～10.8 ×10^-4mol/L and 3.1 ～18.6 ×10^-4 mol/L and the determination limitwas 7.2 ×10^-9 mol/L and 4. 6 ×10^-8 mol/L respectively. This method is simple, rapidand sensitive. The result is accurate.