This article describes synthesis of NiFe2O4 decorated exfoliated graphite particles and its application for pipette tip solid phase extraction of methyl orange (MO) and acid red 18 (AR) dyes from seawater samples prior to their determination by spectrophotometry. Various parameters that effect extraction efficiency such as volume and pH of sample, type and volume of eluent solvent, number of cycles of extraction and elution, type and amount of added salt and concentration of surfactant were investigated and optimized using two methods of one-variable-at-a-time and Box-Behnken response surface methodology. Seven factors in three levels were used for experimental design. Under optimum condition, the linear range of method was 5-250 μg/L for both analytes. The limits of detection achieved were 0.9 and 1.0 μg/L, for MO and AR, respectively. The proposed method was successfully applied for the determination of dyes in seawater samples.