Voltammetric study of 2-guanidinobenzimidazole: Electrode mechanism and determination at mercury electrode

2011 ◽  
Vol 76 (12) ◽  
pp. 1699-1715 ◽  
Author(s):  
Sławomira Skrzypek ◽  
Valentin Mirceski ◽  
Sylwia Smarzewska ◽  
Dariusz Guziejewski ◽  
Witold Ciesielski

Although 2-guanidinobenzimidazole (GBI; CAS: 5418-95-1) is a compound of biological interest, generally there is a lack of electrochemical studies and the methods of its determination. The GBI behavior at a mercury electrode was analyzed under conditions of linear sweep voltammetry (LSV), differential pulse voltammetry (DPV), square-wave voltammetry (SWV) and square-wave stripping voltammetry (SWSV). Although GBI is electrochemically inactive at mercury electrode it adsorbs at the mercury surface and catalyzes effectively the hydrogen evolution reaction. Theoretical analysis of two possible pathways, according to which the GBI electrode mechanism can be explained, is performed. Simple analysis of peak current and potential with respect to available time window, i.e. change of frequency can be helpful in discerning the character of the recorded SW current. The established electrode mechanism is assumed to involve a preceding chemical reaction in which the adsorbed catalyst (GBIads) is protonated and the protonated form of the catalyst (GBIH+(ads)) is irreversibly reduced at potential about –1.18 V vs Ag|AgCl (citrate buffer pH 2.5). New methods of voltammetric determination of 2-guanidinobenzimidazole were developed. The detection and quantifications limits were found to be 1 × 10–7, 1 × 10–6 mol l–1 (SWV); 8 × 10–8, 9 × 10–7 mol l–1 (SWSV); 4 × 10–7, 2 × 10–6 mol l–1 (DPV) and 6 × 10–7, 3 × 10–6 mol l–1 (LSV), respectively.

2004 ◽  
Vol 82 (9) ◽  
pp. 1386-1392 ◽  
Author(s):  
E Hammam ◽  
H S El-Desoky ◽  
K Y El-Baradie ◽  
A M Beltagi

Flutamide is a nonsteriodal anti-androgen drug, which is commonly used in the treatment of advanced prostate cancer. Based on the reduction of the nitro organic moiety of the drug molecule in acetate buffer of pH 5 at the hanging mercury drop electrode, three adsorptive cathodic stripping voltammetric procedures were optimized for determination of flutamide in bulk, tablets, and human serum applying linear-sweep, differential-pulse, and square-wave waveforms. The achieved limits of detection of the bulk drug were 1.9 × 10–7, 8.7 × 10–8, and 9.7 × 10–9 mol L–1 by using the optimized differential-pulse, linear-sweep, and square-wave adsorptive stripping voltammetric procedures, respectively. Repeatability of the results was studied for 1 × 10–6 mol L–1 of the drug and the recoveries obtained were 98.51 ± 1.56% (LSV), 98.89 ± 0.87% (DPV), and 99.21 ± 1.03% (SWV). The proposed procedures were successfully applied to the determination of the drug in pharmaceutical formulation (Eulexin® tablets) and human serum. The detection limits of the drug in bulk, pharmaceutical formulation, and human serum achieved by means of the proposed procedures showed that the square-wave mode was more reliable for determination of the drug especially in its low concentration levels.Key words: flutamide, linear-sweep, differential-pulse, square-wave, cathodic adsorptive stripping voltammetry, determination, Eulexin® tablets, human serum.


2009 ◽  
Vol 12 (13) ◽  
pp. 85-92
Author(s):  
Hien Dinh Thi Nhu Nguyen ◽  
Lam Bich Tran ◽  
Giao Trong Nguyen

A method for trace determination of the pesticide Diazinon using adsorptive square-wave stripping voltammetry (AdSWSV) at the dropping mercury electrode (DME) was described. The pesticide was accumulated at the DME and a well-defined stripping peak was obtained at -1012 mV vs Ag/AgCl/KCI electrode in 0.4 N ammonium acetate electrolyte soluti pH 4.3. Peak current was linear over Diazinon concentration range of 800 – 3200 ppb. Detection limit was 16.49 ppb. Effects of some other pesticides (Chlorpyrifos and Cypermethrin) on Diazinon peak and the recovery of Diazinon from artichoke leaves were studied. The method was extended to the determination of Diazinon in artichoke leaves. The recovery of Diazinon from artichoke leaves was 90.31 - 93.55%. Detection limit was 29.82 ppb. Method had high repeatability and selectivity.


2008 ◽  
Vol 62 (2) ◽  
Author(s):  
Mohammed Ghoneim ◽  
Hanaa El-Desoky ◽  
Mohammed El-Ries ◽  
Ashraf Abd-Elaziz

AbstractTetrazepam dissolved in the Britton-Robinson universal buffer of various pH values (2.5–11.5) containing 10 vol. % of ethanol was reduced at the mercury electrode in a single 2-electron irreversible step due to reduction of the 4,5 C=N double bond of the seven-membered ring. Differential pulse polarography (DPP) and adsorptive cathodic stripping voltammetry (AdCSV) techniques (Linear sweep LS, differential pulse DP and square-wave SW modes) for quantification of tetrazepam in bulk form and in myolastan tablets are presented. Moreover, the described linear sweep, differential pulse, and square-wave adsorptive cathodic stripping voltammetry was successfully applied in quantification of tetrazepam in spiked human serum without any prior extraction of the drug. The obtained results showed an increased sensitivity of the described electro-analytical procedures for the quantification of tetrazepam in the following order DPP, DP-AdCSV, LS-AdCSV, and SW-AdCSV, since the observed limits of tetrazepam quantitation by these electroanalytical techniques were 5 × 10−6 mol L−1, 3 × 10−7 mol L−1, 1 × 10−8 mol L−1, and 3 × 10−9 mol L−1, respectively.


2009 ◽  
Vol 74 (10) ◽  
pp. 1455-1466 ◽  
Author(s):  
Sławomira Skrzypek ◽  
Agnieszka Nosal-Wiercińska ◽  
Witold Ciesielski

Although ganciclovir (gan) as a purine analogue is a compound of biological interest (antiviral drug), it has been rarely electrochemically studied. In this paper surface catalytic electrode mechanism based on the hydrogen evolution reaction is analyzed under conditions of square-wave voltammetry and differential capacity curves of double layer measurements. The electrode mechanism is assumed to involve a preceding chemical reaction in which the adsorbed catalyst (ganads) is protonated at the electrode surface, i.e., ganads + H+aq → ganH+ads. The protonated form of the catalyst (ganH+ads) is irreversibly reduced at potential about –1.35 V vs Ag|AgCl, yielding the initial form of the catalyst and atomic hydrogen, i.e., ganH+ads + e → ganads + Haq. Changes of zero charge potential and surface tension point to the adsorption of ganciclovir molecule directed with guanine group to the mercury surface and suggests that ganciclovir molecules are not placed flat on the mercury surface. The effect of adsorption on mercury electrode was studied in detail in respect to analytical usefulness of the obtained results. A new catalytic method for voltammetric determination of ganciclovir was developed. The detection and quantification limits were 1.3 × 10–7 and 4.3 × 10–7 mol l–1 for square-wave voltammetry, and 1.4 × 10–7 and 4.7 × 10–7 mol l–1 for linear-sweep voltammetry.


2007 ◽  
Vol 5 (3) ◽  
Author(s):  
Amr Beltagi ◽  
Mona El-Attar ◽  
Enass Ghoneim

AbstractThe electro-reduction of tolmetin at the hanging mercury drop electrode was studied in different supporting electrolytes using cyclic voltammetry and square-wave stripping voltammetry techniques. Voltammograms of tolmetin exhibited a single well-defined 2-electron irreversible cathodic peak in media of pH C=O double bond of the analyte molecule. Adsorption of tolmetin onto the surface of the hanging mercury electrode was identified and each adsorbed tolmetin molecule was found to occupy an area of 0.23 nm2. A square-wave adsorptive cathodic stripping voltammetric procedure was described for the direct determination of tolmetin in bulk form and pharmaceutical formulation (Rumatol® capsules) with a limit of quantitation of 2 × 10−9 M and a mean percentage recovery of 98.35 ± 1.21% to 99.57 ± 1.23. Moreover, the described procedure was successfully applied for the direct assay of tolmetin in spiked human serum without pretreatment or extraction prior to the analysis while a quantitation limit of 5 × 10−9 M tolmetin was achieved.


1991 ◽  
Vol 56 (7) ◽  
pp. 1434-1445 ◽  
Author(s):  
Jiří Barek ◽  
Ivana Švagrová ◽  
Jiří Zima

Polarographic reduction of the genotoxic N,N’-dinitrosopiperazine was studied and its mechanism was suggested. Optimum conditions were established for the determination of this substance by tast polarography over the concentration region of 1 . 10-3 to 1 . 10-6 mol l-1 and by differential pulse polarography on the conventional dropping mercury electrode or by fast scan differential pulse voltammetry and linear sweep voltammetry on a hanging mercury drop electrode over the concentration region of 1 . 10-3 to 1 . 10-7 mol l-1. Attempts at increasing further the sensitivity via adsorptive accumulation of the analyte on the surface of the hanging mercury drop failed. The methods are applicable to the testing of the chemical efficiency of destruction of the title chemical carcinogen based on its oxidation with potassium permanganate in acid solution.


2006 ◽  
Vol 71 (11-12) ◽  
pp. 1571-1587 ◽  
Author(s):  
Karel Čížek ◽  
Jiří Barek ◽  
Jiří Zima

The polarographic behavior of 3-nitrofluoranthene was investigated by DC tast polarography (DCTP) and differential pulse polarography (DPP), both at a dropping mercury electrode, differential pulse voltammetry (DPV) and adsorptive stripping voltammetry (AdSV), both at a hanging mercury drop electrode. Optimum conditions have been found for its determination by the given methods in the concentration ranges of 1 × 10-6-1 × 10-4 mol l-1 (DCTP), 1 × 10-7-1 × 10-4 mol l-1 (DPP), 1 × 10-8-1 × 10-6 mol l-1 (DPV) and 1 × 10-9-1 × 10-7 mol l-1 (AdSV), respectively. Practical applicability of these techniques was demonstrated on the determination of 3-nitrofluoranthene in drinking and river water after its preliminary separation and preconcentration using liquid-liquid and solid phase extraction with the limits of determination 4 × 10-10 mol l-1 (drinking water) and 2 × 10-9 mol l-1 (river water).


2017 ◽  
Vol 240 ◽  
pp. 848-856 ◽  
Author(s):  
Mohamad Idris Saidin ◽  
Illyas Md Isa ◽  
Mustaffa Ahmad ◽  
Norhayati Hashim ◽  
Sulaiman Ab Ghani

2013 ◽  
Vol 11 (5) ◽  
pp. 736-741 ◽  
Author(s):  
Robert Piech ◽  
Beata Paczosa-Bator

AbstractThe renewable mercury film electrode, applied for the determination of papaverine traces using differential pulse adsorptive stripping voltammetry (DP AdSV) is presented. The calibration graph obtained for papaverine is linear from 1.25 nM (0.42 µg L−1) to 95 nM (32.2 µg L−1) for a preconcentration time of 60 s, with correlation coefficient of 0.998. For the renewable mercury electrode (Hg(Ag)FE) with a surface area of 9.1 mm2 the detection limit for a preconcentration time of 60 s is 0.7 nM (0.24 µg L−1). The repeatability of the method at a concentration level of the analyte as low as 17 µg L−1, expressed as RSD is 3.3% (n=5). The proposed method was successfully applied and validated by studying the recovery of papaverine from drugs, urine and synthetic solution.


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