Boron-doped multi-walled carbon nanotubes (B-MWCNTs) were synthesized, treated with hydrochloric acid, “piranha” solution, and decorated with gold nanoparticles (AuNPs). B-MWCNTs were characterized using Raman spectroscopy, scanning electron- and transmission electron microscopy, and electrochemical techniques. The results exhibit enhanced response and sensitivity of B-MWCNTs upon modification with AuNPs. Analysis of dopamine (DA) and epinephrine (EP) in presence of uric acid (UA) was investigated on B-MWCNTs/AuNPs in pig blood serum. Limits of detection of 0.20 and 0.30 μM were estimated for DA and EP, respectively. The findings demonstrate that B-MWCNTs/AuNPs is proper for analysis of DA and EP under coexistence of UA.