The aim of this work was to quantify five commonly used pesticides (propoxur, carbaryl, carbendazim,thiabendazole and fuberidazole) in real samples as: tomato, orange juice, grapefruit juice, lemon andtangerine. The method used for the determination of these analytes in the complex matrices washigh-performance liquid chromatography with diode array detection. In order to work under isocraticconditions and to complete each run in less than 10 min, the analysis was carried out applying multi-variate curve resolution coupled to alternating least-squares (MCR?ALS). The flexibility of this appliedmultivariate model allowed the prediction of the concentrations of the five analytes in complex samplesincluding strongly coeluting analytes, elution time shifts, band shape changes and presence of uncali-brated interferents. The obtained limits of detection (in mircog L−1) using the proposed methodology were 2.3 (carbendazim), 0.90 (thiabendazole), 12 (propoxur), 0.46 (fuberidazole) and 0.32 (carbaryl).Fil: Boeris, Valeria. Universidad Nacional de Rosario. Facultad de Ciencias Bioquímicas y Farmacéuticas. Departamento de Química Analítica. Instituto de Química Rosario (IQUIR-CONICET); Argentina.Fil: Arancibia, Juan Alberto. Universidad Nacional de Rosario. Facultad de Ciencias Bioquímicas y Farmacéuticas. Departamento de Química Analítica. Instituto de Química Rosario (IQUIR-CONICET); Argentina.Fil: Olivieri, Alejandro César. Universidad Nacional de Rosario. Facultad de Ciencias Bioquímicas y Farmacéuticas. Departamento de Química Analítica. Instituto de Química Rosario (IQUIR-CONICET); Argentina.