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A novel strategy for optimization of hybrid system of dynamic adsorption/depth filtration. • Fixed bed column/dead-end filtration hybrid separation system was employed for MB removal. • Performance of the hybrid system was optimized using central composite design algorithm. • Feed flowrate was the most affecting variable based on the Pareto sensitivity analysis. • Superiority of the hybrid system performance compared to individual systems at optimum conditions was approved. This work investigates the performance and optimization of a hybrid process consisting of a fixed-bed adsorption (FBA) column and a dead-end filtration (DEF) cell for the removal of methylene blue (MB) from water. Granular activated carbon and cellulose acetate depth filter sheets were used as adsorbent and filter medium, respectively. Effects of four operation parameters (initial concentration, feed flowrate, bed length, and filter type) on the MB removal rate (RR) were investigated using breakthrough data analysis and response surface methodology. This RR (mass of MB removed per second) captures the removal capacity and separation rate, simultaneously. The maximum RR was found theoretically equal to 3.875 s−1 at the optimized conditions of initial concentration =39.86 mg/L, flowrate = 1.15 L/min, bed length =29.95 cm, and filter type = OS100, and validated with the experimental data with 99% agreement. The performance of the hybrid process operating at the optimal operation conditions was found to be superior to those of the individual FBA column and DEF cell. After 100 s from the process commencement, the RR obtained with the hybrid process was about 64% higher than that obtained with the FBA column and 30% higher than that obtained with the DEF cell. [ABSTRACT FROM AUTHOR]