scholarly journals Surface functionalization of natural hydroxyapatite by polymerization of β-cyclodextrin: Application as electrode material for the electrochemical detection of Pb(II)

Author(s):  
Rodrigue Tchoffo ◽  
Guy B. P. Ngassa ◽  
Giscard Doungmo ◽  
Arnaud T. Kamdem ◽  
Ignas Tonle Kenfack ◽  
...  

Abstract A composite material prepared by polymerization of β-cyclodextrin (β-CD) on the surface of natural hydroxyapatite using citric acid as cross linker, was employed as electrode material for the detection of Pb(II). Hydroxyapatite was obtained from bovine bones, following a three-step procedure including pre-calcination, chemical treatment with (NH4)2HPO4 and calcination. The structure of the pristine hydroxyapatite (NHAPP0.5) and its functionalized counterpart (NHAPp0.5-CA-β-CD) materials was examined using XRD and FTIR. Upon deposition as thin film on a glassy carbon electrode (GCE), the ion exchange ability of NHAPp0.5-CA-β-CD was exploited to elaborate a sensitive sensor for the detection of lead. The electroanalytical procedure was based on the chemical accumulation of lead ions under open-circuit conditions, followed by the detection of the preconcentrated species using differential pulse anodic stripping voltammetry. The reproducibility of the proposed method based on different measurements in a solution containing 2 µM lead gave a coefficient of variation of 1.27%. Significant parameters that can affect the lead stripping response were optimized: a linear calibration curve for lead (II) in the concentration range of 2 × 10− 8 mol L− 1 − 20 × 10− 8 mol L− 1 (R2 = 0.998) was obtained. The detection limit (DL = 3S/M) and the sensitivity of the proposed sensor were 5.06 × 10− 10 mol L− 1 and 100.80 µA.µM− 1, respectively. The interfering effect of several ions expected to affect the stripping determination of lead was evaluated, and the proposed sensor was also successfully applied in the determination of Pb2+ ions in spring water and well water.

2019 ◽  
Vol 63 (1) ◽  
Author(s):  
Mehdi Jalali ◽  
Zeinab Deris Falahieh ◽  
Mohammad Alimoradi ◽  
Jalal Albadi ◽  
Ali Niazi

The electrochemical behavior of Bi+3 ions on the surface of a glassy carbon electrode, in acidic media and in the presence of tamoxifen, was investigated. Cyclic voltammetry, chronoamperometry, differential pulse voltammetry, electrochemical impedance spectroscopy, and scanning electron microscopy with energy-dispersive X-ray spectroscopy were used to find the probable mechanism contributing to the reduction of the peak height of bismuth oxidation with an increase in the concentration of tamoxifen. The obtained results show a slight interaction between the bismuth species and tamoxifen which co-deposit on the surface of glassy carbon electrode. Therefore, the reduction in the peak height of bismuth oxidation as a function of tamoxifen concentration was used to develop a new differential pulse anodic striping voltammetry method for determination of trace amount of tamoxifen. The effects of experimental parameters on the in situ DPASV of Bi+3 ions in the presence of tamoxifen shown the optimal conditions as: 2 mol L-1 H2SO4 (1% v v-1 MeOH), a deposition potential of -0.5 V, a deposition time of 60 s, and a glassy carbon electrode rotation rate of 300 rpm. The calibration curve was plotted in the range of 0.5 to 6 µg mL-1 and the limits of detection and quantitation were calculated to be 3.1 × 10-5 µg mL-1 and 1.0 × 10-4 µg mL-1, respectively. The mean, RSD, and relative bias for 0.5 µg mL-1 (n=5) were found to be 0.49 µg mL-1, 0.3%, and 2%, respectively. Finally, the proposed method was successfully used for the determination of tamoxifen in serum and pharmaceutical samples.


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