Métodos eletroanalíticos e cromatográficos aplicados na análise de corantes usados como marcadores em combustíveis

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Estudo da redução eletroquímica e desenvolvimento de métodos eletroanalíticos para a determinação de dicloroacetamidas com atividade antiamebíaca

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Electrochemical Determination of Organic Compounds in Automotive Fuels

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Elucidating Redox-Level Dispersion and Local Dielectric Effects within Electroactive Molecular Films

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Flow injection analysis of free glycerol in biodiesel using a copper electrode as an amperometric detector

The main goal of this work was to develop a simple analytical method for quantification of glycerol based on the electrocatalytic oxidation of glycerol on the copper surface adapted in a flow injection system. Under optimal experimental conditions, the peak current response increases linearly with glycerol concentration over the range 60-3200 mg kg(-1) (equivalent to 3-160 mg L(-1) in solution). The repeatability of the electrode response in the flow injection analysis (FIA) configuration was evaluated as 5% (n = 10), and the detection limit of the method was estimated to be 5 mg kg(-1) in biodiesel (equivalent to 250 mu g L(-1) in solution) (S/N = 3). The sample throughput under optimised conditions was estimated to be 90 h(-1). Different types of biodiesel samples (B100), as in the types of vegetable oils or animal fats used to produce the fuels, were analysed (seven samples). The only sample pre-treatment used was an extraction of glycerol from the biodiesel sample containing a ratio of 5 mL of water to 250 mg of biodiesel. The proposed method improves the analytical parameters obtained by other electroanalytical methods for quantification of glycerol in biodiesel samples, and its accuracy was evaluated using a spike-and-recovery assay, where all the biodiesel samples used obtained admissible values according to the Association of Official Analytical Chemists. Crown Copyright (C) 2011 Published by Elsevier Ltd. All rights reserved.

Direct electroanalytical determination of fluvastatin in a pharmaceutical dosage form: batch and flow analysis

The reduction of luvastatin (FLV) at a hanging mercury-drop electrode (HMDE) was studied by square-wave adsorptive-stripping voltammetry (SWAdSV). FLV can be accumulated and reduced at the electrode, with a maximum peak current intensity at a potential of approximately 1.26V vs. AgCl=Ag, in an aqueous electrolyte solution of pH 5.25. The method shows linearity between peak current intensity and FLV concentration between 1.0 10 8 and 2.7 10 6 mol L 1. Limits of detection (LOD) and quantification (LOQ) were found to be 9.9 10 9 mol L 1 and 3.3 10 8 mol L 1, respectively. Furthermore, FLV oxidation at a glassy carbon electrode surface was used for its hydrodynamic monitoring by amperometric detection in a flow-injection system. The amperometric signal was linear with FLV concentration over the range 1.0 10 6 to 1.0 10 5 mol L 1, with an LOD of 2.4 10 7 mol L 1 and an LOQ of 8.0 10 7 mol L 1. A sample rate of 50 injections per hour was achieved. Both methods were validated and showed to be precise and accurate, being satisfactorily applied to the determination of FLV in a commercial pharmaceutical.

Electroanalytical study of fluvoxamine

Fluvoxamine (FVX) can be reduced at a mercury- drop electrode, with a maximum peak current intensity being obtained at a potential of -0.7 V vs. Ag/ AgCl, in an aqueous electrolyte solution of pH 2. The compound was determined in a pharmaceutical product and in spiked human serum by square-wave adsorptivestripping voltammetry (SWAdSV) after accumulation at the electrode surface, under batch conditions. Because the presence of dissolved oxygen did not interfere significantly with the analysis, it was also possible to determine FVX in the pharmaceutical product by use of a flow-injection analysis (FIA) system with SWAdSV detection. The methods developed were validated and successfully applied to the quantification of FVX in a pharmaceutical product. Recoveries between 76 and 89% were obtained in serum analysis. The FIA– SWAdSV method enabled analysis of up to 120 samples per hour at reduced cost, implying the possibility of competing with the chromatographic methods usually used for this analysis.

Electroanalytical study of the pesticide asulam

The electrochemical behaviour of the herbicide Asulam was studied by cyclic and square wave voltammetry. Asulam may be irreversibly oxidised at a glassy carbon electrode. Maximum currents were obtained at pH=1.9 in aqueous electrolyte solution. Based on the electrochemical behaviour of Asulam, two analytical methodologies were developed for its determination in water samples, using square wave voltammetry (SWV) and flow injection analysis (FIA) coupled with an amperometric detector. Limits of detection of 7.1x10-6 mol L-1 and 1.2x10-8 mol L-1 for SWV and FIA respectively, were achieved. Repeatability was calculated by assessing the relative standard deviation (%) for 10 consecutive determinations of one sample. The found values were 2.1% for SWV and 5.0% for FIA. Validation of the results provided by SWV and FIA methodologies was performed by comparison with results from an HPLC-DAD technique. Good relative deviations were found (<5%). Recovery trials were performed to assess the accuracy of the results and the obtained values were between 84% and 107% for both methods.

Electroanalytical study of the antidepressant sertraline

Aflowinjection squarewave cathodic stripping voltammetric method has been developed for the determination of sertraline in a pharmaceutical preparation. The method shows linearity between peak current intensity and sertraline concentration for the interval between 0.20×10−6 and 1.20×10−6 mol L−1. Limits of detection and quantification were found to be 1.5×10−7 and 5.0×10−7 mol L−1, respectively. Up to 70 samples per hour can be analysed with a good precision (R.S.D. = 2.5%). The proposed method was successfully applied to the determination of sertraline in a commercial product. In the voltammetric determination of sertraline in flow, a high sample rate is obtained at reduced costs, opening the possibility to compete with the chromatographic methods generally used for this analysis.

Electroanalytical Method for the Analysis of Methyldopa In Pharmaceutical Tablets Using a Crude Extract of Laccase from Pycnoporus sanguineus as Oxidizing Agent

Several colorimetric and chromatographic methods have been used for the identification and quantification of methyldopa (MA) in pharmaceutical formulations and clinical samples. However, these methods are time- and reagent-consuming, which stimulated our efforts to develop a simple, fast, and low-cost alternative method. We carried out an electroanalytical method for the determination of MA in pharmaceutical formulations using the crude enzymatic extract of laccase from Pycnoporus sanguineus as oxidizing agent. This method is based on the biochemical oxidation of MA by laccase (LAC), both in solution, followed by electrochemical reduction on glassy carbon electrode surface. This method was employed for the determination of MA in pure and pharmaceutical formulations and compared with the results obtained using the official method. A wide linear curve from 23 x 10(-5) to 1 x 10(-4) mol L(-1) was found with a detection limit calculated from 43 x 10(-6) mol L(-1).

Electroanalytical determination of N-nitrosamines in aqueous solution using a boron-doped diamond electrode

The electrochemical methods cyclic and square-wave voltammetry were applied to develop an electroanalytical procedure for the determination of N-nitrosamines (N-nitrosopyrrolidine, N-nitrosopiperidine and N-nitrosodiethylamine) in aqueous solutions. Cyclic voltammetry was used to evaluate the electrochemical behaviors of N-nitrosamines on boron-doped diamond electrodes. It was observed an irreversible electrooxidation peak located in approximately 1.8 V (vs. Ag/AgCl) for both N-nitrosamines. The optimal electrochemical response was obtained using the following square-wave voltammetry parameters: f = 250 Hz, E(sw) = 50 mV and E(s) = 2 mV using a Britton-Robinson buffer solution as electrolyte (pH 2). The detection and quantification limits determined for total N-nitrosamines were 6.0 x 10(-8) and 2.0 x 10(-7) mol L(-1), respectively.

Electroanalytical determination of bumetanide employing a biomimetic sensor for detection of doping in sports

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Electroanalytical detection of pindolol: comparison of unmodified and reduced graphene oxide modified screen-printed graphite electrodes

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Development of an enzymeless electroanalytical method for the indirect detection of creatinine in urine samples

The aim of this study is to develop a new enzymeless electroanalytical method for the indirect quantification of creatinine from urine sample. This method is based on the electrochemical monitoring of picrate anion reduction at a glassy carbon electrode in an alkaline medium before and after it has reacted with creatinine (Jaffe's reaction). By using the differential pulse voltammetry technique under the optimum experimental conditions (step potential, amplitude potential, reaction time, and temperature), a linear analytical curve was obtained for concentrations of creatinine ranging from 1 to 80 mu mol L-1, with a detection limit of 380 nmol L-1. This proposed method was used to measure creatinine in human urine without the interference of most common organic species normally present in biological fluids (e.g., uric acid, ascorbic acid, glucose, and phosphocreatinine). The results obtained using urine samples were highly similar to the results obtained using the reference spectrophotometric method (at a 95% confidence level). (C) 2012 Elsevier B.V. All rights reserved.

Evaluation Of Different Treatment Methods Against Denture Stomatitis: A Randomized Clinical Study.

The aim of this clinical study was to determine the efficacy of Uncaria tomentosa (cat's claw) against denture stomatitis (DS). Fifty patients with DS were randomly assigned into 3 groups to receive 2% miconazole, placebo, or 2% U tomentosa gel. DS level was recorded immediately, after 1 week of treatment, and 1 week after treatment. The clinical effectiveness of each treatment was measured using Newton's criteria. Mycologic samples from palatal mucosa and prosthesis were obtained to determinate colony forming units per milliliter (CFU/mL) and fungal identification at each evaluation period. Candida species were identified with HiCrome Candida and API 20C AUX biochemical test. DS severity decreased in all groups (P < .05). A significant reduction in number of CFU/mL after 1 week (P < .05) was observed for all groups and remained after 14 days (P > .05). C albicans was the most prevalent microorganism before treatment, followed by C tropicalis, C glabrata, and C krusei, regardless of the group and time evaluated. U tomentosa gel had the same effect as 2% miconazole gel. U tomentosa gel is an effective topical adjuvant treatment for denture stomatitis.