In this study, a solution-processing based galvanic deposition approach is described for in-situ deposition of gold nanoparticles (AuNP) on delaminated titanium Ti3C2Tx nanosheets under ultrasonication. The nanocomposite (AuNP@Ti3C2Tx) was placed on a glassy carbon electrode (GCE) and then applied to electrochemically with label-free, and simultaneously sense uric acid (UA), and folic acid (FA) at physiological pH. The modified GCE has attractive figures of merit: (i) The working potentials for UA and AA are well separated (+0.35V and 0.70V vs. Ag|AgCl); (ii) wide linear responses (from 0.03-1520μM for UA and from 0.02-3580μM for FA; (iii) good electrochemical sensitivities for both UA and FA (0.53 and 0.494μAμM-1.cm-2, respectively), and (iv) detection limits of 11.5nM (UA) and 6.20nM (FA). The electrode exhibited good repeatability (RSD = 4.4%), acceptable reproducibility (RSD = 4.1%), and excellent stability (91.8% over one-month storage). The method was applied to analyze spiked serum samples, and modified GCE is shown appreciable recoveries (97.1-98.8% and 96.8-98.0% for UA, and FA, respectively). Graphical abstractA photograph (top left) of colloidal suspension of gold nanoparticles (AuNPs). They were grown onthe delaminated titanium carbide Ti3C2Tx MXenenanosheet via galvanic displacement deposition method, and their corresponding a low-resolution transmission electron microscopy micrograph (top right) of AuNP@Ti3C2Tx. The graphical representation of AuNP@Ti3C2Tx drop-casted on glassy carbon electrode (GCE) (bottom left), and their voltammetric measurement were applied in the presence of both uric acid and folic acid with increasing the concentration of both analytes (bottom right).