Roberta Antigo Medeiros

Simultaneous voltammetric determination of paracetamol and caffeine in pharmaceutical formulations using a boron-doped diamond electrode.

A simple and highly selective electrochemical method was developed for the single or simultaneous determination of paracetamol (N-acetyl-p-aminophenol, acetaminophen) and caffeine (3,7-dihydro-1,3,7-trimethyl-1H-purine-2,6-dione) in aqueous media (acetate buffer, pH 4.5) on a boron-doped diamond (BDD) electrode using square wave voltammetry (SWV) or differential pulse voltammetry (DPV). Using DPV with the cathodically pre-treated BDD electrode, a separation of about 550 mV between the peak oxidation potentials of paracetamol and caffeine present in binary mixtures was obtained. The calibration curves for the simultaneous determination of paracetamol and caffeine showed an excellent linear response, ranging from 5.0 x 10(-7)mol L(-1) to 8.3 x 10(-5)mol L(-1) for both compounds. The detection limits for the simultaneous determination of paracetamol and caffeine were 4.9 x 10(-7)mol L(-1) and 3.5 x 10(-8)mol L(-1), respectively. The proposed method was successfully applied in the simultaneous determination of paracetamol and caffeine in several pharmaceutical formulations (tablets), with results similar to those obtained using a high-performance liquid chromatography method (at 95% confidence level).

Square-wave voltammetric determination of propranolol and atenolol in pharmaceuticals using a boron-doped diamond electrode

The independent determination of two beta-blocker agents, namely propranolol (PROP) and atenolol (ATN), in pharmaceutical formulations using square-wave voltammetry and a cathodically pretreated boron-doped diamond electrode is described. These electroanalytical determinations of propranolol or atenolol were carried out in 0.1molL(-1) H(2)SO(4) or 0.5molL(-1) NaNO(3) (pH 1.0, adjusted with concentrated HNO(3)), respectively. Excellent linear calibration curves, ranging from 0.20 to 9.0micromolL(-1) for PROP and from 2.0 to 41micromolL(-1) for ATN, with detection limits of 0.18 and 0.93micromolL(-1), respectively, were obtained. The obtained recoveries range from 93.9% to 105.0%, for PROP, and from 92.5% to 106.0%, for ATN. The proposed method was successfully applied in the determination of both beta-blockers in several pharmaceutical formulations (tablets), with results in close agreement at a 95% confidence level with those obtained using official spectrophotometric methods.

Simple Flow Injection Analysis System for Simultaneous Determination of Phenolic Antioxidants with Multiple Pulse Amperometric Detection at a Boron-Doped Diamond Electrode

A method for simultaneous determination of butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) in food was developed that uses multiple pulse amperometry (MPA) with flow injection analysis (FIA). Determination of these phenolic antioxidants was carried out with a cathodically pretreated boron-doped diamond electrode and an aqueous ethanolic (30% ethanol, v/v) 10 mmol L⁻¹ KNO₃ solution (pH(cond) = 1.5) as supporting electrolyte. A dual-potential waveform, at E(det1) = 850 mV/200 ms and E(det2) = 1150 mV/200 ms versus Ag/AgCl (3.0 mol L⁻¹ KCl), was employed. The use of E(det1) or E(det2) caused the oxidation of BHA or of BHA and BHT, respectively; hence, concentration subtraction could be used to determine both species. The respective analytical curves presented good linearity in the investigated concentration range (0.050-3.0 μmol L⁻¹ for BHA and 0.70-70 μmol L⁻¹ for BHT), and the detection limits were 0.030 μmol L⁻¹ for BHA and 0.40 μmol L⁻¹ for BHT. The proposed method, which is simple, quick, and presents good precision and accuracy, was successfully applied in the simultaneous determination of BHA and BHT in commercial mayonnaise samples, with results similar to those obtained by HPLC, at a 95% confidence level.

Simultaneous voltammetric determination of synthetic colorants in food using a cathodically pretreated boron-doped diamond electrode

Differential pulse voltammetry (DPV) and a cathodically pretreated boron-doped diamond (BDD) electrode were used to simultaneously determine two pairs of synthetic food colorants commonly found mixed in food products: tartrazine (TT) and sunset yellow (SY) or brilliant blue (BB) and sunset yellow (SY). In the DPV measurements using the BDD electrode, the reduction peak potentials of TT and SY or BB and SY were separated by about 150 mV. The detection limit values obtained for the simultaneous determination of TT and SY or BB and SY were 62.7 nmol L(-1) and 13.1 nmol L(-1) or 143 nmol L(-1) and 25.6 nmol L(-1), respectively. The novel proposed voltammetric method was successfully applied in the simultaneous determination of these synthetic colorants in food products, with results similar to those obtained using a HPLC method at 95% confidence level.

Square-wave voltammetric determination of acetylsalicylic acid in pharmaceutical formulations using a boron-doped diamond electrode without the need of previous alkaline hydrolysis step

In this paper the determination of acetylsalicylic acid (ASA) in pharmaceutical formulations using square-wave voltammetry (SWV) and a boron-doped diamond electrode (BDD) is described. By this proposed method, ASA is directly determined in a 0.01 mol L-1 H2SO4 solution without the need of a previous time-consuming alkaline hydrolysis step. A single oxidation peak at a potential of 1.97 V vs. Ag/AgCl (3.0 mol L-1 KCl) with the characteristics of an irreversible reaction was obtained. The obtained analytical curve is linear in the ASA concentration range 2.50 × 10-6-1.05 × 10-4 mol L-1, with a detection limit of 2.0 µmol L-1. The obtained relative standard deviation was smaller than 1.4% for a 45 µmol L-1 ASA solution (n = 10). The proposed method was applied with success in the determination of ASA in several pharmaceutical formulations; the obtained results were in close agreement, at a 95% confidence level, with those obtained using an official method of the British Pharmacopoeia.

Simultaneous square-wave voltammetric determination of aspartame and cyclamate using a boron-doped diamond electrode

A simple and highly selective electrochemical method was developed for the simultaneous determination of aspartame and cyclamate in dietary products at a boron-doped diamond (BDD) electrode. In square-wave voltammetric (SWV) measurements, the BDD electrode was able to separate the oxidation peak potentials of aspartame and cyclamate present in binary mixtures by about 400 mV. The detection limit for aspartame in the presence of 3.0x10(-4) mol L(-1) cyclamate was 4.7x10(-7) mol L(-1), and the detection limit for cyclamate in the presence of 1.0x10(-4) mol L(-1) aspartame was 4.2x10(-6) mol L(-1). When simultaneously changing the concentration of both aspartame and cyclamate in a 0.5 mol L(-1) sulfuric acid solution, the corresponding detection limits were 3.5x10(-7) and 4.5x10(-6) mol L(-1), respectively. The relative standard deviation (R.S.D.) obtained was 1.3% for the 1.0x10(-4) mol L(-1) aspartame solution (n=5) and 1.1% for the 3.0x10(-3) mol L(-1) cyclamate solution. The proposed method was successfully applied in the determination of aspartame in several dietary products with results similar to those obtained using an HPLC method at 95% confidence level.

Flow injection simultaneous determination of synthetic colorants in food using multiple pulse amperometric detection with a boron-doped diamond electrode.

A single-line flow injection system and multiple pulse amperometric detection using a boron-doped diamond electrode were employed to develop and optimize a simple, low-cost, and rapid method for the simultaneous determination of two pairs of food colorants: tartrazine and sunset yellow (TT-SY) or brilliant blue and SY (BB-SY). A dual-potential waveform was used: E(det.1)=-150 mV (400 ms duration) and E(det.2)=-450 mV (100 ms duration) vs. Ag/AgCl (3.0 mol L(-1) KCl). Polarization at E(det.1) or E(det.2) causes reduction of SY or the respective pair of colorants, TT-SY or BB-SY; hence, with proper current correction, both colorants in each pair can be determined. The obtained linear response ranges (detection limits) were 5.0-60.0 (2.5) and 1.0-50.0 (0.80) μmol L(-1), for TT and SY, or 5.0-60.0 (3.5) and 1.0-50.0 (0.85) μmol L(-1), for BB and SY, respectively. Investigation of possible interferents (other food colorants or additives) showed no significant interference with the methods here proposed, which were then used to simultaneously determine the pairs of colorants in industrialized food samples, with results that showed good agreement with those obtained using a comparative HPLC method.

Amorphous carbon nitride as an alternative electrode material in electroanalysis: Simultaneous determination of dopamine and ascorbic acid

Boron-doped diamond (BDD) films are excellent electrode materials, whose electrochemical activity for some analytes can be tuned by controlling their surface termination, most commonly either to predominantly hydrogen or oxygen. This tuning can be accomplished by e.g. suitable cathodic or anodic electrochemical pretreatments. Recently, it has been shown that amorphous carbon nitride (a-CNx) films may present electrochemical characteristics similar to those of BDD, including the influence of surface termination on their electrochemical activity toward some analytes. In this work, we report for the first time a complete electroanalytical method using an a-CNx electrode. Thus, an a-CNx film deposited on a stainless steel foil by DC magnetron sputtering is proposed as an alternative electrode for the simultaneous determination of dopamine (DA) and ascorbic acid (AA) in synthetic biological samples by square-wave voltammetry. The obtained results are compared with those attained using a BDD electrode. For both electrodes, a same anodic pretreatment in 0.1 mol L(-1) KOH was necessary to attain an adequate and equivalent separation of the DA and AA oxidation potential peaks of about 330 mV. The detection limits obtained for the simultaneous determination of these analytes using the a-CNx electrode were 0.0656 μmol L(-1) for DA and 1.05 μmol L(-1) for AA, whereas with the BDD electrode these values were 0.283 μmol L(-1) and 0.968 μmol L(-1), respectively. Furthermore, the results obtained in the analysis of the analytes in synthetic biological samples were satisfactory, attesting the potential application of the a-CNx electrode in electroanalysis.

Differential Pulse Voltammetric Determination of Sildenafil Citrate (Viagra®) in Pharmaceutical Formulations Using a Boron-Doped Diamond Electrode

The determination of sildenafil citrate using differential pulse voltammetry and a cathodically pre-treated boron-doped diamond electrode is described. The obtained analytical curve is linear in the sildenafil concentration range 7.3 × 10−7 − 7.3 × 10−6 mol L−1 in a 0.1 mol L−1 H2SO4, with a detection limit of 6.4 × 10−7 mol L−1. The proposed method, which is fast and simple to carry out, was successfully applied in the determination of sildenafil citrate in Viagra® pharmaceutical formulations, with results in close agreement (at 95% confidence level) with those obtained using a comparative HPLC method.

Square‐Wave Voltammetry Determination of Aspartame in Dietary Products Using a Boron‐Doped Diamond Electrode

Abstract The use of square‐wave voltammetry in conjunction with a cathodically pretreated boron‐doped diamond electrode for the analytical determination of aspartame in dietary products is described. In this determination, the samples were analyzed without previous treatment in a 0.5 mol l−1 H2SO4 solution. A single oxidation peak at a potential of 1.6 V vs. Ag/AgCl (3.0 mol l−1 KCl) with the characteristics of an irreversible reaction was obtained. The analytical curve was linear in the aspartame concentration range 9.9×10−6 to 5.2×10−5 mol l−1 with a detection limit of 2.3×10−7 mol l−1. The relative standard deviation (n=5) obtained was smaller than 0.2% for the 1.0×10−4 mol l−1 aspartame solution. The proposed method was applied with success to the determination of aspartame in several dietary products and the results were similar to those obtained using an HPLC method at 95% confidence level.