A multivariate calibration-prediction techniques, principal component artificial neural networks (PCA- ANN) were applied to the spectrometric multicomponent analysis of the drug containing hydrochlorothiazide (HCT) and amiloride hydrochlorothiazide (AMH) without any separation step. The selection of variables was studied. A series of synthetic solution containing different concentrations of HCT and AMH were used to check the prediction ability of the PCA-ANN. The results obtained in this investigation strongly encourage us to apply these techniques for a routine analysis and quality control of the drug.