Abstract: A quantitative method of simultaneous determination of sodium benzenesulfinate and sodium saccharin in nickel plating solution by high performance liquid chromatography has been established. In order to avoid the interference of high salt background in chromatographic analysis, the desalting treatment method of samples was studied. The linearity, recovery and precision of the method were verified, and the actual consumption curves of sodium benzenesulfinate and sodium saccharin in electroplating solution were determined: under a current density of 400 A/m² for 4 h, the average consumption rate of sodium benzenesulfinate was 18.25 mg/h and the average consumption rate of sodium saccharin was 4.05 mg/h. The results showed that the concentration of sodium benzenesulfinate and sodium saccharin had a good linear relationship with the peak area, all the correlation coefficients were greater than 0.993, the spiked recoveries were 91.20%~97.60%, and the relative standard deviations were 2.86%~4.75%. The method is of good repeatability, simple and rapid operation, and is suitable for the detection of two brighters in nickel plating solution.