[Objective] The aim was to explore the cheap,convenient and quick method for simultaneous detection on norfloxacin and ofloxacin.[Method] The spectrum data of the synthetic samples of norfloxacin and ofloxacin was treated and analyzed by four chemometrics methods(CLS,PCR,PLS and RBF-ANN) in the pH=1.81 Britton-Robinson(B-R) buffer solution and the analysis ability of each chemometrics method to the system was discussed.[Result] The linear range of norfloxacin and ofloxacin was 0.6-13.8 mg/L and 0.5-15.0 mg/L,resp.and the detection limit was 0.14 and 0.24 mg/L,resp.The recovery rate of the methods used in the experiment was all between 95% and 105%.The ions likely existed in the practical samples,such as Mg2+ with 300 times,glucose,Zn2+,Ca2+,K+,sodium citrate with 10 times,Fe2+ and Cu2+,could not produced interference on norfloxacin and ofloxacin.The effect of data treated with PCR and PLS was better.[Conclusion] The result of the 2 medicine concn.in the synthetic sample forecasted by the PCR and PLS was better and the method was used to detect the 2 medicine in the plasm of the practical sample,which obtained the better quantitative analysis result.