In this work a numerical method, based on the use of spectrophotometric data coupled to PLS multivariate calibration, is reported for the simultaneous determination of furosemide (FUR) and atenolol (ATE) in synthetic samples and combined commercial tablets. The correlation coefficients (R2) and recovery range for ATE and FUR in synthetic mixtures were 0.9938, 0.9949 and 94.72-103.72%, 95.60-104.34% respectively. The results of optimized method in combined tablet preparations compared with British Pharmacopeia 2007 standard methods that have a good agreement. The proposed method are simple, fast, inexpensive and do not need to any separation or preparation methods.