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A rapid and efficient method for the simultaneous monitoring and recovery of Auramine O (AO) and Methylene Blue (MB) dyes from water samples is presented. This method, named ultrasound-assisted dispersive-magnetic nanocomposites-solid-phase microextraction (UA-DMN-μSPE), utilizes NiCoMn/Fe 3 O 4 @C composite sorbents. Response surface methodology (RSM) combined with artificial neural networks (ANN) and generalized regression artificial neural network (GRNN) under central composite design (CCD) was employed to optimize various parameters for efficient extraction, followed by further refinement using desirability function analysis (DFA) and genetic algorithms (GA). Under optimized conditions, the method achieved exceptional recovery rates (99.5 ± 1.2% for AO and 99.8 ± 1.1% for MB) with acetone as the eluent. Additionally, a high preconcentration factor of 45.50 and 47.30 for AO and MB, respectively, was obtained. Low detection limits of 0.45 ng mL⁻1 (AO) and 1.80 ng mL⁻1 (MB) were achieved with wide linear response ranges (5–1000 and 5–2000 ng mL⁻1 for AO and MB, respectively). The method exhibited good stability with RSDs below 3% for five recycling runs, and minimal interference from various ions was observed. This UA-DMN-μSPE-UV/Vis method offers significant advantages in terms of efficiency, preconcentration, and detection limits, making it a valuable tool for the analysis of AO and MB in water samples. [Display omitted] • UA-DMN-μSPE method optimized using RSM, ANN, and GRNN ensures high-performance MB and AO extraction. • Optimized UA-DMN-μSPE-UV/Vis method, developed with DFA and GA, enhances recovery, preconcentration, and selectivity for MB and AO. • Concurrent monitoring & recovery offers sustainable solution for dye removal. • Potential to address environmental & health concerns from non-degradable dyes. [ABSTRACT FROM AUTHOR]