scholarly journals Nimesulide Determination on Carbon Black-Nafion Modified Glassy Carbon Electrode by Means of Adsorptive Stripping Voltammetry

2021 ◽  
Author(s):  
Marcelina Łysoń ◽  
Anna Górska ◽  
Beata Paczosa-Bator ◽  
Robert Piech

AbstractAdsorptive Stripping Voltammetric method for Nimesulide (NIM) determination was developed. As a working electrode, glassy carbon electrode (GCE) modified with carbon black and Nafion (CB-Nafion GCE) was used. All measurements were carried out in 0.1 M acetate buffer (pH 4.6). Conducted experiments allowed to optimize differential pulse voltammetry (DPV) instrumental parameters: sampling and waiting time ts = tw = 10 ms, step potential Es = 4 mV, and pulse amplitude ΔE = 50 mV. The best results were obtained for preconcentration potential and time equal to 400 mV and 20 s, respectively. Limit of detection was calculated and was equal to 0.14 µM for 20-s preconcentration time and 0.06 µM for 40-s preconcentration time. In order to prove the applicability of the developed method, concentration of nimesulide in pharmaceutical products was determined. Calculated recoveries were in the range 94–99%, which indicates that the method might be assumed as accurate. Coefficient of variation was equal to 5.0% (n = 7, NIM concentration 1 µM) Obtained results of NIM determination were in good agreement with the content declared by producers.

Sensors ◽  
2020 ◽  
Vol 21 (1) ◽  
pp. 60
Author(s):  
Anna Górska ◽  
Beata Paczosa-Bator ◽  
Robert Piech

A new, highly sensitive Adsorptive Stripping Voltammetric method for levodopa determination was developed. As a working electrode, the glassy carbon electrode (GCE) modified with carbon black (CB), RuO2·xH2O (RuO2) and Nafion was used (CB-RuO2-Nafion GCE). Levodopa signal obtained on the modified electrode was 12 times higher compared to GCE. During research, instrumental parameters were optimized: sampling time ts = 10 ms, waiting time tw = 10 ms, step potential Es = 5 mV and pulse amplitude ΔE = 50 mV. Preconcentration potential Eprec was equal to 0 mV. The best results were obtained in 0.025 M perchloric acid (approx. pH 1.4). Signal repeatability measured on the CB-RuO2-Nafion modified electrode for 0.2 µM of levodopa was equal to 2.1% (levodopa concentration 1 µM, n = 5). Linearity of the method was achieved in the concentration range from 1 to 8 µM. Limit of detection was equal to 17 nM. Recoveries calculated for pharmaceutical products and tap water measurements were in the range 102–105%, which confirms the accuracy of the developed. The applicability of the method was confirmed by analysis of pharmaceutical products and tap water samples. Based on obtained results, it might be concluded that the developed voltammetric method could be a useful tool in routine drug analysis.


Materials ◽  
2021 ◽  
Vol 14 (24) ◽  
pp. 7582
Author(s):  
Izabela Bargiel ◽  
Joanna Smajdor ◽  
Anna Górska ◽  
Beata Paczosa-Bator ◽  
Robert Piech

A new voltametric method for highly sensitive propranolol (PROP) determination was developed. A glassy carbon electrode modified with a hybrid material made of carbon black (CB) and Nafion was used as the working electrode. The preconcentration potential and time were optimized (550 mV and 15 s), as well as the supporting electrolyte (0.1 mol L−1 H2SO4). For 15 s preconcentration time, linearity was achieved in the range 0.5–3.5 μmol L−1 and for 120 s in 0.02–0.14 μmol L−1. Based on the conducted calibration (120 s preconcentration time) limit of detection (LOD) was calculated and was equal to 7 nmol L−1. To verify the usefulness of the developed method, propranolol determination was carried out in real samples (tablets and freeze-dried urine). Recoveries were calculated and were in the range 92–102%, suggesting that the method might be considered as accurate. The repeatability of the signal expressed as relative standard deviation (RSD) was equal to 1.5% (n = 9, PROP concentration 2.5 µmol L−1). The obtained results proved that the developed method for propranolol determination might be successfully applied in routine laboratory practice.


2018 ◽  
Vol 4 (5) ◽  
pp. 567-571
Author(s):  
Aaron Mary Ratna Sylvia ◽  
C. Vedhi ◽  
A. Gomathi

The voltammetric behaviour of 4-nitroso-N,N–dimethylaniline (4-NDMA) was investigated on plain glassy carbon electrode (GCE) and multi-walled carbon nanotube modified GCE (MWCNT/GCE) using cyclic voltammetry. Effects of pH, scan rate and concentration were studied. The surface morphology of the modified electrode in the absence and presence of 4-NDMA molecules was characterized by atomic force microscope (AFM). A systematic study on the variation of experimental parameters with differential pulse stripping voltammetry (DPSV) was carried out and the optimized experimental conditions were arrived. MWCNT/GCE performed well compared with the plain GCE system and the limit of detection (LOD) was found to be 7.5 ng/mL 0.1056 ng/mL for 4-NDMA on plain GCE and MWCNT/GCE respectively.


Nanomaterials ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 1266
Author(s):  
Aftab A. Khand ◽  
Saeed A. Lakho ◽  
Aneela Tahira ◽  
Mohd Ubaidullah ◽  
Asma A. Alothman ◽  
...  

Recently, the oxidative behavior of methotrexate (MTX) anticancer drug is highly demanded, due to its side effects on healthy cells, despite being a very challenging task. In this study, we have prepared porous NiO material using sodium sulfate as an electronic disorder reagent by hydrothermal method and found it highly sensitive and selective for the oxidation of MTX. The synthesized NiO nanostructures were characterized by scanning electron microscope (SEM) and X-ray diffraction (XRD) techniques. These physical characterizations delineated the porous morphology and cubic crystalline phase of NiO. Different electrochemical approaches have been utilized to determine the MTX concentrations in 0.04 M Britton–Robinson buffer (BRB) at pH 2 using glassy carbon electrode (GCE)-modified with electronically disordered NiO nanostructures. The linear range for MTX using cyclic voltammetry (CV) was found to be from 5 to 30 nM, and the limit of detection (LOD) and limit of quantification (LOQ) were 1.46 nM and 4.86 nM, respectively, whereas the linear range obtained via linear sweep voltammetry (LSV) was estimated as 15–90 nM with LOD and LOQ of 0.819 nM and 2.713 nM, respectively. Additionally, amperometric studies revealed a linear range from 10 to70 nM with LOD and LOQ of 0.1 nM and 1.3 nM, respectively. Importantly, MTX was successfully monitored in pharmaceutical products using the standard recovery method. Thus, the proposed approach for the synthesis of active metal oxide materials could be sued for the determination of other anticancer drugs in real samples and other biomedical applications.


2021 ◽  
Vol 12 (1) ◽  
Author(s):  
Pattan-Siddappa Ganesh ◽  
Ganesh Shimoga ◽  
Seok-Han Lee ◽  
Sang-Youn Kim ◽  
Eno E. Ebenso

Abstract Background A simple and simultaneous electrochemical sensing platform was fabricated by electropolymerization of allura red on glassy carbon electrode (GCE) for the interference-free detection of dihydroxy benzene isomers. Methods The modified working electrode was characterized by electrochemical and field emission scanning electron microscopy methods. The modified electrode showed excellent electrocatalytic activity for the electrooxidation of catechol (CC) and hydroquinone (HQ) at physiological pH of 7.4 by cyclic voltammetric (CV) and differential pulse voltammetric (DPV) techniques. Results The effective split in the overlapped oxidation signal of CC and HQ was achieved in a binary mixture with peak to peak separation of 0.102 V and 0.103 V by CV and DPV techniques. The electrode kinetics was found to be adsorption-controlled. The oxidation potential directly depends on the pH of the buffer solution, and it witnessed the transfer of equal number of protons and electrons in the redox phenomenon. Conclusions The limit of detection (LOD) for CC and HQ was calculated to be 0.126 μM and 0.132 μM in the linear range of 0 to 80.0 μM and 0 to 110.0 μM, respectively, by ultra-sensitive DPV technique. The practical applicability of the proposed sensor was evaluated for tap water sample analysis, and good recovery rates were observed. Graphical abstract Electrocatalytic interaction of ALR/GCE with dihydroxy benzene isomers.


Materials ◽  
2021 ◽  
Vol 14 (4) ◽  
pp. 723
Author(s):  
Kgotla K. Masibi ◽  
Omolola E. Fayemi ◽  
Abolanle S. Adekunle ◽  
Amal M. Al-Mohaimeed ◽  
Asmaa M. Fahim ◽  
...  

This report narrates the successful application of a fabricated novel sensor for the trace detection of endosulfan (EDS). The sensor was made by modifying a glassy-carbon electrode (GCE) with polyaniline (PANI), chemically synthesized antimony oxide nanoparticles (AONPs), acid-functionalized, single-walled carbon nanotubes (fSWCNTs), and finally, the AONP-PANI-SWCNT nanocomposite. The electrochemical properties of the modified electrodes regarding endosulfan detection were investigated via cyclic voltammetry (CV) and square-wave voltammetry. The current response of the electrodes to EDS followed the trend GCE-AONP-PANI-SWCNT (−510 µA) > GCE-PANI (−59 µA) > GCE-AONPs (−11.4 µA) > GCE (−5.52 µA) > GCE-fSWCNTs (−0.168 µA). The obtained results indicated that the current response obtained at the AONP-PANI-SWCNT/GCE was higher with relatively low overpotential compared to those from the other electrodes investigated. This demonstrated the superiority of the AONP-PANI-SWCNT-modified GCE. The AONP-PANI-SWCNT/GCE demonstrated good electrocatalytic activities for the electrochemical reduction of EDS. The results obtained in this study are comparable with those in other reports. The sensitivity, limit of detection (LoD), and limit of quantification (LoQ) of AONP-PANI-SWCNT/GCE towards EDS was estimated to be 0.0623 µA/µM, 6.8 µM, and 20.6 µM, respectively. Selectivity, as well as the practical application of the fabricated sensor, were explored, and the results indicated that the EDS-reduction current was reduced by only 2.0% when interfering species were present, whilst average recoveries of EDS in real samples were above 97%.


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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