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This work presents for the first time the systematic preparation of a novel carbon nanotube-MCM-41 hybrid employing the mesoporous material MCM-41 as a successful dispersant for multiwall carbon nanotubes (MWCNTs). Relevant dispersion variables such as the amount of MWCNTs, MCM-41 concentration, and sonication time were optimized through a central composite design (CDD)/response surface methodology (RSM). Several solvents were evaluated and N,N-dimethylformamide (DMF) was selected because it allowed reaching stable dispersions with very good electrochemical response. The electrochemical performance of glassy carbon electrodes (GCE) modified with different hybrids was evaluated by cyclic voltammetry (CV) using ascorbic acid (AA) as redox marker, while their surface morphology was characterized by SEM microscopy. The optimal MWCNT–MCM-41 dispersion condition was 0.75 mg mL−1 MWCNTs, 0.25 mg mL−1 MCM-41, and 30 min sonication. Both, electrochemical results and SEM images correlate with a percolation behavior from MWCNT–MCM-41 hybrid. Electrooxidation of AA at GCE modified with the optimal hybrid occurred under diffusion control and exhibited an enhanced current response (65 μA) and a lower overvoltage (−0.005 V) compared to bare GCE (ip = 22 μA, Ep = 0.255 V). The amperometric response of AA at GCE/MWCNT–MCM-41 exhibited remarkable figures of merit, including an ultralow detection limit (1.5 nM), high sensitivity (45.4 × 103 μA M−1), excellent short- and long-term stability, and very good anti-interference ability for AA detection. The analytical applicability of the developed electrochemical sensor was evaluated by sensing AA in several real samples, showing excellent correlation with the values reported by manufacturers in both pharmaceutical and food samples. [ABSTRACT FROM AUTHOR]