In the present work, a simple and economic analytical method based on attapulgite/nafion coated glassy carbon electrode (AT/Naf/GCE) has been developped for the electrochemical determination of caffeine. Prior to its use, the ionic exchange properties and conductivity of AT/Naf/GCE were studied by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). Caffeine gave an irreversible oxidation peak around +1.41 V (vs Ag/AgCl reference electrode) in 0.1 M H2SO4 at pH 1.5. The peak current varied linearly with the square root of the scan rate, showing that the transfer process is controlled by diffusion. The heterogeneous rate constant, the transfer coefficient and the number of electrons involved were calculated. Upon optimization of key analytical parameters involved in the electroanalysis of caffeine by DPV, the recorded oxidation peak current varied linearly with caffeine concentration in the range from 0.1 to 4 μm, leading to a detection limit of 4.57×10−8 M (S/N=3). The developed electrode exhibited good stability and was easily regenerated. The effect of some important potential interfering compounds (ascorbic acid, dopamine, uric acid, sulphite ions and glucose) on the signal of caffeine was also examined. The obtained electrode was successfully employed in the determination of caffeine content in a commercial drug.
Herein, a convenient method based on a fullerene/multiwalled carbon nanotube/Nafion modified glassy carbon electrode (fullerene/MWCNT/Naf/GCE) for the electrochemical determination of caffeine (CAF) is reported. Cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) were used to study ionic exchange properties and conductivity the proposed electrode using [Fe(CN) 6 ] 3−/4− redox couple. Caffeine gave an irreversible oxidation peak around +1.33 V (vs. Ag/AgCl reference electrode) in HClO 4 (pH 1). The linear dependence of the peak current with the square root of the scan rate showed that the electron transfer process is controlled by diffusion. After optimization of key analytical parameters involved in differential pulse voltammetry (DPV), the oxidation peak current varied linearly with CAF concentration in the range of 10 to 1000 µM. A detection limit of 7.289 × 10 −8 M (S/N = 3) was found. Kinetic and chronocoulometric studies were also performed to characterize the diffusion of CAF. The developed electrode exhibited good stability and was easily regenerated. The influence of some potential interfering compounds such as dopamine, uric acid, glucose and sulfite ions on the anodic peak current of CAF was also examined. The proposed method was successfully employed in the determination of CAF in some commercial drugs.
An electrochemical sensor was prepared by modification of glassy carbon electrode (GCE) with an organoclay obtained by intercalation of smectite-type clay Sa(Na) with dimethydioctadecylammonium ions (DODAB) and polymer of alizarin red S (poly [ARS]). The synthesized materials were analyzed by physicochemical and electrochemical techniques. The fabricated sensor GCE/Sa (DODAB)/poly(ARS) was employed toward the detection of diuron and the detection limit was found to be 0.48 μM (0.11 mg/L). Additionally, the elaborated electrochemical sensor was found to exhibit good sensitivity, stability, and reproducibility toward the determination of diuron, and it was applied successfully in real samples.
An amperometric sensor was developed by depositing a film coating of hydroxyapatite (HA)/L-lysine (Lys) composite material on a glassy carbon electrode (GCE). It was applied for the detection of Nile blue A (NBA). Hydroxyapatite was obtained from snail shells and its structural properties before and after its combination with Lys were characterized using X-ray diffraction (XRD), Fourier-transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), and Brunauer–Emmett–Teller (BET) surface area analyses. The coupling of Lys to HA was attributed to favorable interaction between negatively charged -COO− groups of Lys and divalent ions Ca2+ of HA. Electrochemical investigations pointed out the improvement in sensitivity of the GCE/Lys/HA sensor towards the detection of NBA in solution. The dependence of the peak current and potential on the pH, scan rate, and NBA concentration was also investigated. Under optimal conditions, the GCE/Lys/HA sensor showed a good reproducibility, selectivity, and a NBA low detection limit of 5.07 × 10−8 mol L−1. The developed HA/Lys-modified electrode was successfully applied for the detection of NBA in various water samples.
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