In this study, ultrasound-assisted dispersive solid phase micro-extraction based on nanosorbent namely silver-zinc oxide nanoparticles loaded on activated carbon (Ag-ZnO-NP-AC) combined with derivative spectrophotometry method for the simultaneous pre-concentration and determination of Methyl Green (MG) and Rose Bengal (RB) dyes in water and industrial wastewater. Characterized sorbent by field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX), particle-size distribution (PSD), Fourier transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD) and Transmission electron microscopy (TEM) analysis with superior adsorption capacity was applied in ultrasound assisted dispersive-solid-phase micro-extraction (UA-DSPME) methodology. pH, sorbent mass, ultrasonication time, and eluent volume influence and contribution on response correspond to simultaneous pre-concentration and determination of MG and RB were optimized by response surface methodology (RSM) and results were compared with the experimental values. Under the optimal conditions (UA-DSPME), the enrichment factors (EFs) were 93.89 and 97.33 for the MG and RB dyes, respectively. The limits of detection were 2.14 and 2.73ngmL−1 and the limit of quantification were 7.15 and 9.09ngmL−1 for MG and RB, respectively. The analytes can be determined over 10–2000ngmL−1 with recoveries between 90.8% to 97.7% and RSDs less than 3.6%. The developed method due to simplicity and rapidity is able successful for repeatable and accurate monitoring of under study analytes from complicated matrices.