Herein, we investigated the electrochemical behaviour of fMWCNTs decorated with Co-Nd bimetallic nanoparticles and alumina nanoparticles (Co-Nd/Al
2
O
3
@fMWCNTs). The nanocomposites were synthesised using simple mechanical mixing and characterised by FT-IR, XRD, UV–visible studies, SEM, TEM and EDAX. Moreover, the crystalline size of the synthesised nanoparticles was also calculated using XRD data (Debye–Scherer formula) and was found in the nm range. The electrochemical behaviour of epinephrine (EP) was examined in the presence of Co-Nd/Al
2
O
3
@fMWCNTs nanocomposite modified glassy carbon electrode (GCE) using various electrochemical techniques such as cyclic voltammetry (CV), differential pulse voltammetry (DPV), electrochemical impedance spectroscopy (EIS), and chronocoulometry. Among all the above-mentioned techniques, the DPV response of the modified Co-Nd/Al
2
O
3
@fMWCNTs/GCE under optimal circumstances revealed a dual linear range (0.2 to 4000 µM and 4000 to 14,000 µM) and LOD of 0.015 µM (
S
/
N
= 3). The sensitivities were determined to be 0.00323 µAµM
−1
and 0.0004 µAµM
−1
in 0.2 to 4000 µM and 4000 to 14,000 µM concentration ranges. Using chronocoulometry, the surface coverage of Co-Nd/Al
2
O
3
@fMWCNTs/GCE was calculated to be 1.37 × 10
−8
mol cm
−2
. The fabricated Co-Nd/Al
2
O
3
@fMWCNTs/GCE demonstrated remarkable repeatability, with an RSD of 0.09%, and storage stability of 3 weeks, with 89.6% current retention. Lastly, it was found that Co-Nd/Al
2
O
3
@fMWCNTs/GCE worked well for EP analysis in a variety of biological fluids.
Graphical abstract
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