In this study, models were developed for the simultaneous determination of Benazepril (BEN) and hydrochlorothiazide (HCT) in drug samples using chemometric approaches using UV spectrophotometry. It was used to calculate the calibration mixes between 200 and 360 nm wavelengths at 5 nm intervals for the spectra of BEN and HCT at various concentrations. The least squares calibration method and principal component regression were used for chemometric analysis of the data and the parameters of the chemometric procedures were optimized. The analytical performances of this chemometric method were compared by characterizing the sum of the residual errors' squares (PRESS), estimated standard error (SEP) and recoveries (%). A series of synthetic mixtures containing different concentrations of BEN and HCT were studied to control the predictive ability of the chemometric methods applied. This method was successfully applied to real samples, it was not affected by excipients as stated in the recovery study results. The results obtained in this review encourage these chemometric methods to apply these strategies for standard research and quality control of two active ingredients.