A partial least-squares calibration (PLS) method has been developed for simultaneous quantitative determination of mepyramine maleate (MAM), lidocaine hydrochloride (LIH), and dexpanthenol (DPA) in pharmaceutical preparations. The resolution of these mixtures has been accomplished by using partial least-squares (PLS-2) regression analysis of electronic absorption spectral data without prior separation or derivatization. The experimental calibration matrix was constructed with 27 samples. The concentration ranges considered were 2, 3, 4 µg mL -1 for MAM, 2, 3, 4 µg mL -1 for LIH, and 8, 10, 12 µg mL -1 for DPA. The absorbances were recorded between 190 and 340 nm every 5 nm. The results show that PLS-2 is a simple, rapid, and accurate method applied to the determination of these compounds in pharmaceuticals. [ABSTRACT FROM AUTHOR]