Adsorptive Voltammetric Studies on the Cerium(III)–Alizarin Complexon Complex at a Carbon Paste Electrode

A novel procedure was developed for the determination of trace cerium on the basis of anodic adsorption voltammetry of the Ce(III)–alizarin complexon (ALC) complex at a carbon paste electrode (CPE). The procedure is convenient to determine cerium individually in the presence of other rare earths because there is a 100 mV difference between the peak potentials of Ce(III)–ALC and other rare earth(III)–ALC complexes in a supporting electrolyte of 0.08 M HAc–NaAc and 0.012 M potassium biphthalate (pH 4.7) when performing linear-scanning from −0.2 to 0.8 V (vs. SCE) at 100 mV/s. The second-order derivative peak currents are directly proportional to the Ce(III) concentration over a range of 6.0 × 10⁻⁹–3.0 × 10⁻⁷ M. The detection limit is as low as 2.0 × 10⁻⁹ M (S/N = 3) for a 120 s preconcentration. An RSD of 3.5% was obtained for 15 determinations of Ce(III) at a concentration of 4.0 × 10⁻⁸ M on the same CPE surface. The method was applied successfully to the determination of cerium in samples of rare earth nodular graphite cast iron.     

Adsorptive anodic stripping voltammetry of zirconium(IV)-alizarin red S complex at a carbon paste electrode

A sensitive adsorptive anodic stripping procedure for the determination of trace zirconium at a carbon paste electrode (CPE) has been developed. The method is based on adsorptive accumulation of the Zr(IV)-alizarin red S(ARS) complex onto the surface of the CPE, followed by oxidation of adsorbed species. The optimal experimental conditions include the use of 0.10 mol · L⁻¹ ammonium acetate buffer (pH 4.3), ARS, an accumulation potential of 0.20 V (versus SCE), an accumulation time of 2 min, a scan rate of 200 mV · s⁻¹ and a second-order derivative linear scan mode. The oxidation peak for the complex appears at 0.69 V. The peak current is proportional to the concentration of Zr(IV) over the range of 1.0 × 10⁻⁹–2.0 × 10⁻⁷ mol · L⁻¹, and the detection limit is 3 × 10⁻¹⁰ mol · L⁻¹ for a 2 min adsorption time. The relative standard deviations (n = 8) for 5.0 × 10⁻⁸ and 5.0 × 10⁻⁹ mol · L⁻¹ Zr(IV) are 3.3 and 4.8%, respectively. The proposed method was applied to the determination of zirconium in ore samples with satisfactory results.     

Electrochemical determination of lead(II) using a montmorillonite calcium-modified carbon paste electrode

Utilizing the fascinating properties of montmorillonite calcium (MMT-Ca), such as huge cationic exchange capacity, strong adsorptive ability, high chemical and mechanical stability, an MMT-Ca modified carbon paste electrode (CPE) was constructed for the sensitive determination of Pb²⁺. In 0.01 mol·L⁻¹ HCl, Pb²⁺ was firstly exchanged and accumulated on an MMT-Ca modified CPE surface and secondly reduced to Pb at −0.90 V. In the following potential sweep from −0.90 to −0.50 V, reduced Pb was oxidized, resulting in an obvious stripping peak at −0.58 V. After optimizing the parameters, such as determining medium, content of MMT-Ca, accumulation potential and time, an electrochemical method was developed for the analysis of Pb²⁺. Compared with bare CPE, the MMT-Ca modified CPE significantly enhances the sensitivity of Pb²⁺ analysis. The limit of detection is evaluated to be 6.0 × 10⁻⁹ mol L⁻¹ Pb²⁺. Finally, this method was successfully employed to determine trace levels of Pb²⁺ in water samples. The first two authors contribute equally do this work     

Simultaneous and sensitive determination of procaine and its metabolite for pharmaceutical quality control and pharmacokinetic research by using a graphite paste electrode

A simple, rapid, sensitive, and accurate method for simultaneous electrochemical determination of procaine and its metabolite (p-aminobenzoic acid, PABA) for pharmaceutical quality control and pharmacokinetic research was developed using a graphite paste electrode. The differential pulse voltammetric results revealed that procaine and p-aminobenzoic acid, respectively, showed well-defined anodic oxidation peaks on a carbon paste electrode with a current peak separation of 155 mV at a scan rate of 100 mV s⁻¹. This well separation of the current peaks for these two compounds in voltammetry enables us to simultaneously determine them. Good linearity (r > 0.998) between oxidation peak current and concentration was obtained in the range of 5.0 × 10⁻⁷–5.0 × 10⁻⁵ M for procaine and 5.0 × 10⁻⁷–2.0 × 10⁻⁵ M for PABA in pH 4.50 acetate buffer solution. The detection limit for both analytes is 5 × 10⁻⁸ M (S/N = 3:1). The present voltammetric method has been successfully used to determine trace p-aminobenzoic acid in procaine hydrochloride injection and procaine in plasma with a linear relationship of current to its concentration ranging from 1.0 × 10⁻⁶ to 5.0 × 10⁻⁵ M (correlation coefficient of 0.9981) with a low detection limit of 5.0 × 10⁻⁷ M (S/N = 3:1). This validated method is promising to the study of pharmacokinetics in Sprague–Dawley rat and rabbit plasma after an intravenous administration of procaine hydrochloride injection.     

Electrochemical deposition of silicate–cetyltrimethylammonium bromide nanocomposite film on glassy carbon electrode for sensing of methyl parathion

A novel electrochemical sensor for methyl parathion based on silicate– cetyltrimethylammonium bromide nanocomposite film has been fabricated by electro-assisted deposition onto glassy carbon electrode in one-step via an electrochemical modulation of pH at the electrode/solution interface to promote controlled gelification of tetraethylorthosilicate sol, and was characterized with scanning electron microscopy, X-ray diffraction, and electrochemical impedance spectroscopy. The electrochemical sensing of methyl parathion on the film-modified electrode was investigated applying cyclic voltammetry and square wave voltammetry. Compared to the unmodified electrode, the shapes of the redox peaks were improved and the peak currents significantly increased. Experimental parameters such as deposition time, pH value, and accumulation conditions have been optimized. A linear relationship between the peak current and methyl parathion concentration was obtained in the range from 1.0 × 10⁻⁷ to 1.0 × 10⁻⁴ mol L⁻¹ with a detection limit of 1.04 × 10 ⁻⁸ mol L⁻¹ (S/N = 3) after accumulation at 0 V for 120 s. The film electrode shows great promise for determination of methyl parathion in real samples.      

Voltammetric sensor for nitrite determination based on its electrocatalytic reduction at the surface of p-duroquinone modified carbon paste electrode

A p-duroquinone (tetramethyl-p-benzoquinone) modified carbon paste electrode (DMCPE) was employed to study the electrocatalytic reduction of nitrite in aqueous solutions using cyclic voltammetry (CV), double potential-step chronoamperometry, and differential pulse voltammetry (DPV). It has found that under an optimum condition (pH 1.00), the reduction of nitrite at the surface of DMCPE occurs at a potential of about 660 mV less negative than that of an unmodified carbon paste electrode (CPE). The catalytic rate constant, k′_h, based on Andrieux and Saveant theoretical model was calculated as for scan rate 10 mV s^-1. Also, the apparent diffusion coefficient, D _app, was found as 2.5 × 10^–10 and 3.61 × 10^–5 cm² s^-1 for p-duroquinone in carbon paste matrix and nitrite in aqueous buffered solution, respectively. The values for αn_α were estimated to be −0.65 and −0.19 for the reduction of nitrite at the surface of DMCPE and CPE, respectively. The electrocatalytic reduction peak currents showed a linear dependence on the nitrite concentration, and a linear analytical curve was obtained in the ranges of 5.0 × 10^–5 M to 8.0 × 10^–3 M and 6.0 × 10^–6 M to 8.0 × 10^–4 M of nitrite concentration with CV and DPV methods, respectively. The detection limits (2σ) were determined as 2.5 × 10^–5 M and 4.3 × 10^–6 M by CV and DPV methods. This method was also applied as a simple, selective and precise method for determination of nitrite in real samples (the weak liquor from the wood and paper factory of Mazandaran province in Iran) by using a standard addition method.     

Electrochemical Study of 4-Nitrophenol at a Modified Carbon Paste Electrode

 A zeolite-modified carbon paste electrode (CPE) has been used for the determination of 4-nitrophenol by differential pulse voltammetry (DPV). The electrochemical reduction of 4-nitrophenol at −1.0 V is carried out in a Britton-Robinson medium at pH 3.5. The cyclic voltammetric (CV) behaviour has been investigated to study the nature of the process. Studies on the effect of pH were carried out over the pH range 2–9 with the Britton-Robinson buffer solution, and the influence of pH on peak height and peak potential was analyzed. A linear relationship between peak intensity and concentration is obtained in the range 0.2–10 mg L⁻¹, with a detection limit of 0.04 mg L⁻¹; a relative standard deviation of 1.5% for a 5 mg L⁻¹ 4-nitrophenol concentration and a relative error of 2.6% were also obtained (n=11). Received March 3, 1998. Revision December 10, 1998.     

Electrochemical characterization of 2, 2′-[1, 2-ethanediylbis (nitriloethylidyne)]-bis-hydroquinone-carbon nanotube paste electrode and its application to simultaneous voltammetric determination of ascorbic acid and uric acid

The preparation and electrochemical characterization of a carbon nanotube paste electrode modified with 2,2′-[1,2-ethanediylbis (nitriloethylidyne)]-bis-hydroquinone, referred to as EBNBH, was investigated. The EBNBH carbon nanotube paste electrode (EBNBHCNPE) displayed one pair of reversible peaks at E _pa = 0.18 V and E _pc = 0.115 V vs Ag/AgCl. Half wave potential (E _1/2) and ΔE _p were 0.148 and 0.065 V vs Ag/AgCl, respectively. The electrocatalytic oxidation of ascorbic acid (AA) has been studied on EBNBHCNPE, using cyclic voltammetry, differential pulse voltammetry and chronoamperometry techniques. It has been shown that the oxidation of AA occurs at a potential where oxidation is not observed at the unmodified carbon paste electrode. The heterogeneous rate constant for oxidation of AA at the EBNBHCNPE was also determined and found to be about 1.07 × 10⁻³ cm s⁻¹. The diffusion coefficient of AA was also estimated as 5.66 × 10⁻⁶ cm² s⁻¹ for the experimental conditions, using chronoamperometry. Also, this modified electrode presented the property of electrocatalysing the oxidation of AA and uric acid (UA) at 0.18 and 0.35 V vs Ag/AgCl, respectively. The separations of anodic peak potentials of AA and UA reached 0.17 V. Using differential pulse voltammetry, the calibration curves for AA and UA were obtained over the range of 0.1–800 μM and 20–700 μM, respectively. With good selectivity and sensitivity, the present method provides a simple method for selective detection of AA and UA in biological samples.     

Simple sensor for simultaneous determination of dihydroxybenzene isomers

A simple sensor based on bare carbon ionic liquid electrode was fabricated for simultaneous determination of dihydroxybenzene isomers in 0.1 mol L⁻¹ phosphate buffer solution (pH 6.0). The oxidation peak potential of hydroquinone was about 0.136 V, catechol was about 0.240 V, and resorcinol 0.632 V by differential pulse voltammetric measurements, which indicated that the dihydroxybenzene isomers could be separated absolutely. The sensor showed wide linear behaviors in the range of 5.0 × 10⁻⁷–2.0 × 10⁻⁴ mol L⁻¹ for hydroquinone and catechol, 3.5 × 10⁻⁶–1.535 × 10⁻⁴ mol L⁻¹ for resorcinol, respectively. And the detection limits of the three dihydroxybenzene isomers were 5.0 × 10⁻⁸, 2.0 × 10⁻⁷, 5.0 × 10⁻⁷ mol L⁻¹, respectively (S/N = 3). The proposed method could be applied to the determination of dihydroxybenzene isomers in artificial wastewater and the recovery was from 93.9% to 104.6%.     

Electrochemical behavior and determination of epinephrine at a mercaptoacetic acid self-assembled gold electrode

The electrochemical behavior of epinephrine (EP) at a mercaptoacetic acid (MAA) self-assembled monolayer modified gold electrode was studied. The MAA/Au electrode is demonstrated to promote the electrochemical response of epinephrine by cyclic voltammetry. The possible reaction mechanism is also discussed. The diffusion coefficient D of EP is 6.85 × 10⁻⁶ cm² s⁻¹. In 0.1 mol L⁻¹ phosphate buffer (pH 7.20), a sensitive oxidation peak was observed at 0.177 V, and the peak current is proportional to the concentration of EP in the range of 1.0 × 10⁻⁵–2.0 × 10⁻⁴ mol L⁻¹ and 1.0 × 10⁻⁷–1.0 × 10⁻⁶ mol L⁻¹. The detection limit is 5 × 10⁻⁸ mol L⁻¹. The modified electrode is highly stable and can be applied to the determination of EP in practical injection samples. The method is simple, quick, sensitive and accurate.     

Analysis of domperidone in pharmaceutical formulations and wastewater by differential pulse voltammetry at a glassy-carbon electrode

The redox characteristics of the drug domperidone at a glassy-carbon electrode (GCE) in aqueous media were critically investigated by differential-pulse voltammetry (DPV) and cyclic voltammetry (CV). In Britton–Robinson (BR) buffer of pH 2.6–10.3, an irreversible and diffusion-controlled oxidation wave was developed. The dependence of the CV response of the developed anodic peak on the sweep rate (ν) and on depolizer concentration was typical of an electrode-coupled chemical reaction mechanism (EC) in which an irreversible first-order reaction is interposed between the charges. The values of the electron-transfer coefficient (α) involved in the rate-determining step calculated from the linear plots of E _p,a against ln (ν) in the pH range investigated were in the range 0.64 ± 0.05 confirming the irreversible nature of the oxidation peak. In BR buffer of pH 7.6–8.4, a well defined oxidation wave was developed and the plot of peak current height of the DPV against domperidone concentration at this peak potential was linear in the range 5.20 × 10⁻⁶ to 2.40 × 10⁻⁵ mol L⁻¹ with lower limits of detection (LOD) and quantitation (LOQ) of 6.1 × 10⁻⁷ and 9.1 × 10⁻⁷ mol L⁻¹, respectively. A relative standard deviation of 2.39% (n = 5) was obtained for 8.5 × 10⁻⁶ mol L⁻¹ of the drug. These DPV procedures were successfully used for analysis of domperidone in the pure form (98.2 ± 3.1%), dosage form (98.35 ± 2.9%), and in tap (97.0 ± 3.6%) and wastewater (95.0 ± 2.9%) samples. The method was validated by comparison with standard titrimetric and HPLC methods. Acceptable error of less than 3.3 % was also achieved. Figure In aqueous media at pH 7.6- 8.4, the DPV and cyclic voltammetry of the drug domperidone (I) at GCE showed an irreversible and diffusion controlled oxidation wave. The values of the electron transfer coefficient (α) involved in the rate determining step were found in the range 0.64± 0.05 confirming the irreversible nature of the peak. The analysis of the drug in pure form and in wastewater samples was successfully achieved     

Electrochemistry and electrocatalytic activity of polypyrrole/ferrocyanide films on a glassy carbon electrode

Functionalized polypyrrole films were prepared by incorporation of Fe(CN)₆ ³⁻ as doping anion during the electropolymerization of pyrrole at a glassy carbon electrode from aqueous solution. The electrochemical behavior of the Fe(CN)₆ ³⁻/Fe(CN)₆ ⁴⁻ redox couple in polypyrrole was studied by cyclic voltammetry. An obvious surface redox reaction was observed and dependence of this reaction on the solution pH was illustrated. The electrocatalytic ability of polypyrrole film with ferrocyanide incorporated was demonstrated by oxidation of ascorbic acid at the optimized pH of 4 in a glycine buffer. The catalytic effect for mediated oxidation of ascorbic acid was 300 mV and the bimolecular rate constant determined for surface coverage of 4.5 × 10⁻⁸ M cm⁻² using rotating disk electrode voltammetry was 86 M⁻¹ s⁻¹. Furthermore, the catalytic oxidation current was linearly dependent on ascorbic acid concentration in the range 5 × 10⁻⁴–1.6 × 10⁻² M with a correlation coefficient of 0.996. The plot of i _p versus v ^1/2 confirms the diffusion nature of the peak current i _p. Received: 12 April 1999 / Accepted: 25 May 1999     

Electrochemical methods for simultaneous determination of trace amounts of dopamine and uric acid using a carbon paste electrode incorporated with multi-wall carbon nanotubes and modified with α-cyclodextrine

In this work, we investigate the electrochemical activity of dopamine (DA) and uric acid (UA) using both a bare and a modified carbon paste electrode as the working electrode, with a platinum wire as the counter electrode and a silver/silver chloride (Ag/AgCl) as the reference electrode. The modified carbon paste electrode consists of multi-walled carbon nanotubes (>95%) treated with α-cyclodextrine, resulting in an electrode that exhibits a significant catalytic effect toward the electro-chemical oxidation of DA in a 0.2-M Britton–Robinson buffer solution (pH 5.0). The peak current increases linearly with the DA concentration within the molar concentration ranges of 2.0 × 10⁻⁶ to 5.0 × 10⁻⁵ M and 5.0 × 10⁻⁵ to 1.9 × 10⁻⁴ M. The detection limit (signal to noise >3) for DA was found to be 1.34 × 10⁻⁷ M, respectively. In this work, voltammetric methods such as cyclic voltammetry, chronoamperometry, chronocuolometry, differential pulse and square wave voltammetry, and linear sweep and hydrodynamic voltammetry were used. Cyclic voltammetry was used to investigate the redox properties of the modified electrode at various scan rates. The diffusion coefficient (D, cm² s⁻¹ = 3.05 × 10⁻⁵) and the kinetic parameters such as the electron transfer coefficient (α = 0.51) and the rate constant (k, cm³ mol⁻¹ s⁻¹ = 1.8 × 10³) for DA were determined using electrochemical approaches. By using differential pulse voltammetry for simultaneous measurements, we obtained two peaks for DA and UA in the same solution, with the peak separation approximately 136 mV. The average recovery was measured at 102.45% for DA injection.     

Adsorption voltammetry of the zirconium-alizarin red S complex at a multi-walled carbon nanotubes modified carbon paste electrode

We used a carbon paste electrode modified with multi-walled carbon nanotubes as a working electrode and studied the electrochemical behavior of zirconium-alizarin red S complex on it. It was found that the modified electrode exhibited a significant catalytic effect toward the reduction of free alizarin red S and the complex. The second derivative linear scan voltammograms of the complex were recorded by a polarographic analyser from 0 to −1000 mV (vs. SCE), and it was found that the complex can be adsorbed on the surface of the modified electrode, yielding a peak at about −470 mV, corresponding to the reduction of alizarin red S in the complex. The linear range was found to be 2.0 × 10⁻¹¹–8.0 × 10⁻⁷ mol L⁻¹, and the detection limit was 1.0 × 10⁻¹¹ mol L⁻¹ (S/N = 3) for 3 min accumulation. The procedure was successfully applied to the determination of trace amounts of zirconium in the ore samples. Correspondence: Pei-Hong Deng, Department of Chemistry and Material Science, Hengyang Normal University, Hengyang Hunan 421008, P.R. China     

Voltammetric Sensor for the Determination of Parathion Using an Electropolymerized Poly(Carmine) Film Electrode

A voltammetric sensor for the determination of parathion has been developed based on the use of a poly(carmine) film electrode. The reduction of parathion at the poly(carmine) modified glassy carbon electrode (GCE) is studied by cyclic voltammetry (CV) and linear scan voltammetry (LSV). Parathion yields a well-defined reduction peak at a potential of −0.595 V on the poly(carmine) modified GCE in pH 6.0 phosphate buffer solution (PBS). Compared with that on a bare GCE, the reduction peak current of parathion is significantly enhanced. All the experimental parameters are optimized for the determination of parathion. The reduction peak current is linear with the parathion concentration in the range of 5.0 × 10⁻⁸ to 1.0 × 10⁻⁵ mol L⁻¹, and the detection limit is 1.0 × 10⁻⁸ mol L⁻¹.     

Electrochemistry and voltammetric determination of tannic acid on a single-wall carbon nanotube-coated glassy carbon electrode

The voltammetric behavior of tannic acid (TA) on a single-wall carbon nanotubes (SWNTs) modified glassy carbon electrode has been investigated by cyclic voltammetry. TA can generate a well-defined anodic peak on the modified electrode at around 0.42 V (vs. SCE) in 0.10 M phosphate buffer solutions (pH = 4.0). The electrochemical reaction involves 1e transfer, accompanied by one proton. The electrode process is controlled by adsorption. The parameters affecting the response of TA, such as solution pH, accumulation time and accumulation potential are optimized for the determination of TA. Under the optimum conditions, the peak current changes linearly with the TA concentration in the range of 5.0 × 10⁻⁸–1.0 × 10⁻⁶ M. The lowest detectable concentration of TA is 8.0 × 10⁻⁹ M after 180 s accumulation. This method has been successfully applied to the determination of TA in tea and beer samples. In addition, the influence of potential interferents is examined. In the presence of bovine serum albumin, the peak current of TA decreases linearly due to the formation of a super-molecular complex.     

A New Differential Pulse Voltammetric Method for the Determination of Nitrate at a Copper Plated Glassy Carbon Electrode

 A differential pulse voltammetric method for the determination of nitrate has been described, which is applicable to the analysis of natural water samples with nitrate levels greater than 2.8 × 10⁻⁶ M. A reduction peak for the nitrate ions at a freshly copper plated glassy carbon electrode was observed at about −0.50 V vs Ag ∣AgCl∣KCl_satd electrode in a solution of 2.0 × 10⁻² M Cu²⁺, 0.5 M H₂SO₄ and 1.0 × 10⁻³ M KCl and exploited for analytical purposes. The working linear range was established by regression analysis and found to extend from 2.8 ×10⁻⁶ M to 8.0 × 10⁻⁵ M. The proposed method was applied for the determination of nitrate in natural waters. The detection limit of the method was 2.8 × 10⁻⁶ M and the sensitivity was 0.9683 A·L/mol. The possible interferences by some ions such as phosphate, nitrite and some halides were determined and found to lead to shifts of the peak position and increasing the peak heights. Received March 15, 1999. Revision July 9, 1999.     

Simultaneous determination of phenylenediamine isomers and dihydroxybenzene isomers in hair dyes by capillary zone electrophoresis coupled with amperometric detection

The simultaneous determination of three isomers of phenylenediamines (o, m, and p-phenylenediamine) and two isomers of dihydroxybenzenes (catechol and resorcinol) in hair dyes was performed by capillary zone electrophoresis coupled with amperometric detection (CZE–AD). The effects of working electrode potential, pH and concentration of running buffer, separation voltage, and injection time on CZE–AD were investigated. Under the optimum conditions the five analytes could be perfectly separated in 0.30 mol L⁻¹ borate–0.40 mol L⁻¹ phosphate buffer (pH 5.8) within 15 min. A 300 μm diameter platinum electrode had good responses at +0.85 V (versus SCE) for the five analytes. Their linear ranges were from 1.0 × 10⁻⁶ to 1.0 × 10⁻⁴ mol L⁻¹ and the detection limits were as low as 10⁻⁷ mol L⁻¹ (S/N = 3). This working electrode was successfully used to analyze eight kinds of hair dye sample with recoveries in the range 91.0–108.0% and RSDs less than 5.0%. These results demonstrated that capillary zone electrophoresis coupled with electrochemical detection using a platinum working electrode as detector was convenient, highly sensitive, highly repeatable and could be used in the rapid determination of practical samples. Figure Electropherograms obtained from 10 mg mL⁻¹ hair dye sample solutions at a platinum working electrode under optimum CZE–AD conditions: (a) natural black (I), (b) golden: (1) p-phenylenediamine, (2) m-phenylenediamine, (3) o-phenylenediamine, (4) resorcinol, and (5) catechol     

FAD-modified SiO2/ZrO2/C ceramic electrode for electrocatalytic reduction of bromate and iodate

SiO₂/ZrO₂/C carbon ceramic material with composition (in wt%) SiO₂ = 50, ZrO₂ = 20, and C = 30 was prepared by the sol–gel-processing method. A high-resolution transmission electron microscopy image showed that ZrO₂ and the graphite particles are well dispersed inside the matrix. The electrical conductivity obtained for the pressed disks of the material was 18 S cm⁻¹, indicating that C particles are also well interconnected inside the solid. An electrode modified with flavin adenine dinucleotide (FAD) prepared by immersing the solid SiO₂/ZrO₂/C, molded as a pressed disk, inside a FAD solution (1.0 × 10⁻³ mol L⁻¹) was used to investigate the electrocatalytic reduction of bromate and iodate. The reduction of both ions occurred at a peak potential of −0.41 V vs. the saturated calomel reference electrode. The linear response range (lrr) and detection limit (dl) were: BrO₃ ⁻, lrr = 4.98 × 10⁻⁵–1.23 × 10⁻³ mol L⁻¹ and dl = 2.33 μmol L⁻¹; IO₃ ⁻, lrr = 4.98 × 10⁻⁵ up to 2.42 × 10⁻³ and dl = 1.46 μmol L⁻¹ for iodate.     

Electroreduction and Quantification of Furazolidone and Furaltadone in Different Media

 Adsorptive cathodic stripping voltammetry was used for the determination of furazolidone (FZ) and furaltadone (FD) in borax and phosphate buffers, respectively, using HMDE as working electrode. The influence of different factors upon the peak current response such as accumulation potential, scan rate, preconcentration time, pH and other variables was studied. Furazolidone and furaltadone showed an adsorption character on HMDE in presence of borax and phosphate buffers, respectively. A single cathodic peak at −0.36 V in borax (pH = 9.5) was observed for FZ, while FD gave a cathodic peak at −0.32 V in phosphate buffer (pH = 8.5). The calibration graph showed a linear behavior over the range 3×10⁻⁹–9×10⁻⁸ mol dm⁻³ for furazolidone. In the case of FD, concentrations from 3×10⁻⁹ to 2×10⁻⁷ mol dm⁻³ gave a linear relationship with the peak current. A detection limit of 2×10⁻⁹ mol dm⁻³ and 1×10⁻⁹ mol dm⁻³ was obtained for furazolidone and furaltadone, respectively. This method was applied to determine these drugs in pharmaceutical formulations, urine and serum samples. Received December 15, 1998. Revision February 4, 2000.