This study investigates the non-enzymatic electrochemical sensing of bisphenol A (BPA) in drinking water and milk using a bimetallic nickel-copper pyridine-2,6-dicarboxylic acid (PDA) metal-organic framework (Ni-Cu(PDA)MOF) anchored on carbon nanofiber paper (CNF). The Ni-Cu(PDA)MOF/CNF hybrid material is highly porous, hydrophilic, and has a large surface area, facilitating easy analyte molecule access and enhancing sensitivity. The modified glassy carbon electrode (Ni-Cu(PDA)MOF/CNF/GCE) exhibits good catalytic activity and strong electrochemical sensitivity toward BPA, with a linear range from 1 to 150 μmol/L and a low limit of detection (LOD) of 75 n mol/L. The sensor shows excellent anti-interference properties, reproducibility, and storage stability for up to one month. The Ni-Cu(PDA)MOF/CNF/GCE successfully detected BPA in milk and drinking water samples, with satisfactory results confirmed by chromatographic analysis. This study highlights the potential of bimetallic MOFs in developing sensitive and reliable electrochemical sensors for environmental and food safety applications.This study investigates the non-enzymatic electrochemical sensing of bisphenol A (BPA) in drinking water and milk using a bimetallic nickel-copper pyridine-2,6-dicarboxylic acid (PDA) metal-organic framework (Ni-Cu(PDA)MOF) anchored on carbon nanofiber paper (CNF). The Ni-Cu(PDA)MOF/CNF hybrid material is highly porous, hydrophilic, and has a large surface area, facilitating easy analyte molecule access and enhancing sensitivity. The modified glassy carbon electrode (Ni-Cu(PDA)MOF/CNF/GCE) exhibits good catalytic activity and strong electrochemical sensitivity toward BPA, with a linear range from 1 to 150 μmol/L and a low limit of detection (LOD) of 75 n mol/L. The sensor shows excellent anti-interference properties, reproducibility, and storage stability for up to one month. The Ni-Cu(PDA)MOF/CNF/GCE successfully detected BPA in milk and drinking water samples, with satisfactory results confirmed by chromatographic analysis. This study highlights the potential of bimetallic MOFs in developing sensitive and reliable electrochemical sensors for environmental and food safety applications.