ZnFe (PBA)@Mo3C2Tx is prepared by in‐situ sonication method using ZnFe Prussian blue analogue infused with Mo3C2Tx (MXene) to use as a non‐enzymatic glucose sensor owing to its low cost and biocompatibility. The synthesized ZnFe (PBA)@Mo3C2Tx is characterized for its physical and chemical characterization by XRD, Raman, XPS, EDAX, and FESEM analyses, revealing a functionalized multiple‐layered structure with a cubic nano‐hybrid arrangement. This sensor has undergone electroanalytical investigation, including cyclic voltammetry and chronoamperometry analysis. The electrochemical performance of ZnFe(PBA)@Mo3C2Tx exhibits an excellent analytical performance with a sensitivity of 818.285 μA mM−1 cm−2 and the limit of detection (LOD) of 1.6 μM (S/N=3). The analysis of glucose in human sweat samples, compared with their corresponding blood glucose values, yield a relative standard deviation (RSD) of 2.98 %.