A simple and highly sensitive electrochemical sensor was developed for adsorptive cathodic stripping voltammetry of alprazolam. Based on an electrochemically pretreated glassy carbon electrode, the sensor demonstrated good adsorption and electrochemical reduction of alprazolam. The morphology of the glassy carbon electrode and the electrochemically pretreated glassy carbon electrode were characterized by scanning electron microscopy/energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, cyclic voltammetry, and electrochemical impedance spectroscopy. The electrochemical behaviors of alprazolam were determined by cyclic voltammetry, and the analytical measurements were studied by adsorptive cathodic stripping voltammetry. Optimized operational conditions included the concentration and deposition time of sulfuric acid in the electrochemical pretreatment, preconcentration potential, and preconcentration time. Under optimal conditions, the developed alprazolam sensor displayed a quantification limit of 0.1 mg L−1, a detection limit of 0.03 mg L−1, a sensitivity of 67 µA mg−1 L cm−2 and two linear ranges: 0.1 to 4 and 4 to 20 mg L−1. Sensor selectivity was excellent, and repeatability (%RSD < 4.24%) and recovery (82.0 ± 0.2 to 109.0 ± 0.3%) were good. The results of determining alprazolam in beverages with the developed system were in good agreement with results from the gas chromatography–mass spectrometric method.
Using a simple method, a glassy carbon electrode was electrochemically pretreated for highly sensitive determination of clonazepam. The electrochemically pretreated glassy carbon electrode was employed as an adsorbent and a working electrode for the detection of clonazepam by adsorptive cathodic stripping voltammetry. The surface morphology and electrochemical properties of the glassy carbon electrode and the electrochemically pretreated glassy carbon electrode were studied by energy dispersive X-ray spectroscopy and cyclic voltammetry. The analytical measurements of clonazepam were evaluated using adsorptive cathodic stripping voltammetry. To obtain the optimal electrochemical reduction of clonazepam by the electrochemically pretreated glassy carbon electrode, the electrochemical pretreatment process, preconcentration potential and preconcentration time were optimized. The detection of clonazepam standards under the optimal conditions produced a cathodic current response with a detection limit of 19 μg l−1, quantification limit of 63 μg l−1 and a linear range from 0.0250 to 1.50 mg l−1. The sensor exhibited excellent sensitivity (453 μA mg−1 l cm−2), and good repeatability (%RSD < 11%) and recovery (98 ± 2 to 102 ± 4%). The developed sensor was successfully utilized for the measurement of clonazepam in beverage samples.
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