In this study, the simultaneous quantitative analysis of Cefadroxil, Cefixim in tablets using multivarite linear regression based on near infrared spectral has been developed. The same model of partial least squares (PLS) with 6 separate vector matrix is built with standard matrix of samples (22 samples containing 4 analytes together with total of excipients) were applied for individual and/or simultaneous determination of Cefadroxil, Cefixim in samples. A matrix of test samples including 10 samples created by known amount of components was used to assess the accuracy of the PLS model. The results indicated the relative error varied from 1.1 to 15%. The optimum experimental conditions were spectral region: 3600 - 2800 cm-1
volume ratio of sample/ KBr 2/98 (w/w)
15 mg of pellet form. The analytical results of 2 commercial drug samples containing 1 of 2 actives by means of near-infrared spectral and chromatographic methods HPLC mass spectrometry showed the small relative error (Keywords: Near-infrared method, linear regression, partial least squares, HPLC