A 3D cobalt metal−organic framework (Co−MOF), [Co3(BDC)3(DMU)2], was utilized to prepare Cu@Co−MOF composite in a deposition−reduction process. Cu@Co−MOF/GCE (GCE = glassy carbon electrode) electrode was prepared by "drop−coating" method. Cu@Co−MOF/GCE shows excellent electrocatalytic activity for Glu detection. The chronoamperometric response of Cu@Co−MOF/GCE to Glu concentration (CGlu) displays linear relationships in two CGlu sections with calculated sensitivities of 282.89 μA mM−1 cm−2

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... n 0.005–0.4 mM Glu and 113.15 μA mM−1 cm−2 within 0.4–1.8 mM Glu. The detection limit is calculated as 1.6 μM at S/N = 3. Cu@Co−MOF/GCE also exhibits a rapid current response, high anti−interference, stability, and repeatability to Glu detection. Cu@Co−MOF/GCE was applied to detect Glu in human serum and orange juice. All found CGlu are very close to those added CGlu with low RSDs and high recoveries. Cu@Co−MOF/GCE as a non−enzymatic electrochemical sensor of Glu has high sensitivity, selectivity, accuracy, and reliability.