In the present study, new nano-adsorbents were prepared from the walnut (WSN) and almond (ASN) shells for the sequestering of aflatoxin B-1 (AFB(1)) contamination. The nano-adsorbents were characterized via SEM, EDS, XRD, and FTIR spectroscopy techniques to discover valuable data about the morphology, surface, and chemical configuration of the nano-adsorbents. The adsorption process was further optimized by altering the biosorbent dosage, AFB(1) concentration, pH, time, and temperature. Among the tested biosorbents, the WSN and ANS presented a significant removal of AFB(1 )compared with the walnut and almond shell powders (WSP and ASP). The maximum removal using WSN and ASN was achieved as 93.70% and 83.81% using 10 mg/mL of nano-adsorbent, pH 5.0 at 45 degrees C for 45 min. Langmuir was the best fitting model for each adsorption data with adsorption capacities of WSP, ASP, WSN, and ASN were 47.6, 36.1, 176.3, and 161.1 mg/g, respectively, with a leading monolayer form adsorption. Kinetic data followed the pseudo-second-order with fast AFB(1) uptake. However, thermodynamics studies indicated the spontaneity and endothermic nature of the adsorption process. Furthermore, no significant decline in AFB(1) adsorption was recorded after reusability up to five times. The production of nano-adsorbents in this study offers the possibility of dropping the cost of production, controlling agro-waste, and reducing toxins and other organic materials. Finally, the adsorption presentation confirmed the ability of this novel, cost-effective, environment-friendly, and non-toxic biosorbent to remove AFB(1) effectively.