For the purpose of removing methylene blue (MB) from various ecological water samples, a brand-new solid phase micro-extraction in portable syringe system (SPME-PSS) has been developed. A 100 cm long by 5 mm wide column containing 10 mg of Poly(3-hydroxy butyrate)-b-Poly(methyl methacrylate) with Ag nanoparticles (PHB-AgPrici) serving as the adsorbent PHB-surface AgPrici's morphology has been studied using DSC, FT-IR, and SEM-EDX techniques. Adsorption mechanism of MB toward PHB-AgPrici was investigated using isotherms, kinetics, and thermodynamics experiments. To test adsorption and the capacity of PHB-AgPrici for adsorption, Langmuir and Freundlich's isotherms method was utilized. It was anticipated for MB to have a 169.3 mg/g monolayer adsorption capacity (qmax) toward PHB-AgPrici. The proposed sorbent material could successfully be recycled ten times (via adsorption and desorption cycles) without losing any of its capacity for regeneration. A kinetic analysis was also conducted, and it was discovered that the reaction obeyed pseudo-second-order kinetics because of a higher R2 and good qe values. The Kf and 1/n values (1/n > 0.1) further adhered to the favorable nature of adsorption. The G° (-3.7093) and H° (4.40391) values indicate that the reaction should be endothermic, but the S° (25.107698) data indicate that there is unpredictability at the solid solution interface throughout the adsorption phase. A multivariate optimization methodology was utilized to progress a superior considerate of the synergistic connection between the extraction and separation procedures by concentrating on the optimization of extraction parameters. Central composite design (CCD) was utilized for optimization procedure variables of PHB-AgPrici and (cycle of adsorption/desorption) later combining optimization. The recommended technique offers a linear reaction for MB over the range of conc. 10 to 150 µg L− 1 with correlation coefficient ≥ 0.99775. Validity of the desired approach has been confirmed by spiking addition technique. The recommended technique was productively utilized to diverse real water samples. Furthermore, based on the experimental results, a mechanism is proposed for the adsorptive removal of organic dyes with PHB-AgPrici polymer adsorbent.