Novel bismuth nanoparticle-modified mesoporous carbon (MPC) was successfully prepared on a glassy carbon electrode (Bi@MPC/GCE) for the adsorptive stripping voltammetric determination of nickel by complexing with dimethylglyoxime (DMG). The presence of MPC obviously improved the properties of Bi particles like the electron transfer ability, particle size and hydrophicility, important parameters to achieve preferable analytical performances of Bi@MPC/GCE toward Ni(II). The best electrochemical behaviors of Bi@MPC/GCE was obtained for the stripping determination of Ni(II), compared with electrodes individually modified with Bi and MPC. The synergic effect between metallic Bi and ordered MPC (forming a 3D array like Bi microelectrodes) made major contribution to such improved electrochemical properties of Bi@MPC/GCE for Ni(II) sensing. The good linear analytical curve was achieved in a Ni(II) concentration range from 0.1[Formula: see text][Formula: see text]M to 5.0[Formula: see text][Formula: see text]M with a correlation coefficient of 0.9995. The detection limit and sensitivity were calculated to be 1.2[Formula: see text]nM ([Formula: see text]) and 1410[Formula: see text][Formula: see text]A[Formula: see text]mM[Formula: see text][Formula: see text]cm[Formula: see text], respectively. The new method was successfully applied to Ni(II) determination in soybean samples with recoveries higher than 99% and proved to be a simple, efficient alternative for Ni(II) monitoring in real samples.
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