The present work explores synthesis of a nano-porous network of DMTD-Ag coordination polymer derived from 2,5-Dimercapto-1,3,4-thiadiazole (DMTD) and AgNO3. This network of DMTD-Ag is thoroughly investigated using FT-IR, Raman, XPS, SEM, TEM and TGA. After that a successful application of DMTD-Ag for the electrochemical assay of atropine sulphate using differential pulse voltammetry (DPV) technique, demonstrates the effectiveness of its excellent conducting matrix. The effective structure of DMTD-Ag favors the channeling of electron by providing a large surface area and effective support for the proficient oxidation of atropine sulphate. The anodic peak current showed a linear dependence with concentration of atropine sulphate with sensitivity and limit of detection as 0.02 mu A/mu M and 46.00 nM, respectively. Further the proof of concept is utilized in the assay of atropine sulphate present in clinical formulation (eye drop) with a sensitivity of 0.02 mu A/mu M, and limit of detection as 72.50 nM. (C) 2015 Elsevier Ltd. All rights reserved.