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The early detection of abnormal levels of purine derivatives such as xanthine (XA) and uric acid (UA) in the body fluid could be helpful to prevent various diseases. A novel free-standing biosensor electrode was fabricated by solvothermal deposition of sea-urchin-like cobalt(benzene 1,3,5-tricarboxylic acid)MOF (Co(TMA)MOF) on the surface of electrospun porous carbon nanofibers (CNFs) and explored for the electrochemical detection of XA and UA in the alkaline medium (pH ∼13). The morphological and textural features of the as-fabricated Co(TMA)MOF@CNF hybrid mat were evaluated. The electrochemical investigation of the Co(TMA)MOF@CNF electrode demonstrated an excellent electrocatalytic response toward the selective detection of XA and UA. The diffusion-controlled electrooxidation reactions of XA and UA were identified. The calibration plots of amperometric current response vs analyte …