Análise screening de vinhos empregando um analisador fluxo-batelada, espectroscopia UV-VIS e quimiometria

A simple, robust, versatile, high analytical frequency method was proposed to check if a sample of wine is within the range of standards set by the manufacturer, using the UV-VIS spectroscopy, multivariate analysis and a flow-batch analyzer. Two hundred and fifty-two samples of wines were analyzed. The results from the application of Hierachical Cluster Analysis (HCA) to the matrix of the data involving all samples show the formation of fifteen types of wine. A Soft Independent Modelling of Class Analogy (SIMCA) model was constructed and used to classify the samples of the overall forecast. As a result, it is observed that the prediction was performed with a success rate of 99.2% for a confidence level of 95%. This shows that the proposed methodology can be used as an effective tool for classifying of samples of wines.

Desenvolvimento de um método reflectométrico ambientalmente mais amigável para a determinação de metoclopramida em formulações farmacêuticas

A simple and more environmentally friendly method by combined spot test-diffuse reflectance spectroscopy for determining metoclopramide in pharmaceutical formulations is described. The method is based on the reaction between metoclopramide and p-dimethylaminocinnamaldehyde, in the presence of HCl, producing a colored compound (λmáx = 580 nm) on the filter paper. The linear range was from 5.65 x 10-4-6.21x10-3 mol L-1 (r = 0.999). The limit of detection was 1.27 x 10-4 mol L-1. The proposed reflectometric method was applied successfully to the determination of metoclopramide in pharmaceuticals and it was favorably compared with the Brazilian or British Pharmacopoeia methods at 95% confidence level.

Determination of 5-aminosalicylic acid in pharmaceutical formulations by square wave voltammetry at pencil graphite electrodes

An analytical method for the determination of the anti-inflammatory drug 5-aminosalicylic acid (5-ASA) in pharmaceutical formulations using square wave voltammetry at pencil graphite electrodes was developed. After the optimization of the experimental conditions, calibration curves were obtained in the linear concentration range from 9.78 × 10-7 to 7.25 × 10-5 mol L-1 resulting in a limit of detection of 2.12 ± 0.05 x 10-8 mol L-1. Statistical tests showed that the concentrations of 5-ASA in commercial tablets and enemas obtained with the proposed voltammetric method agreed with HPLC values at a 95% confidence level.

Utilização de planejamento fatorial no preparo de amostras de detergente em pó para a determinação de fósforo por análise em fluxo

The decomposition of detergent powder samples in a microwave oven and autoclave was evaluated. To establish the best experimental conditions a 2(5) factorial design was performed, varying the conditions in autoclave and microwave digestion and flow system parameters for the determination of phosphorus. The best composition was: 0.2 mL sulfuric acid; 500 W power and a 2 min time interval; 6 mmol L-1 of ascorbic acid and 16 mmol L-1 of molybdate to flow system. This factor levels use less reagents than the reference method. No statistically significant differences were found between the autoclave and microwave oven responses at the 95% confidence level.

Sequential injection analysis system with spectrophotometric detection for determination of norfloxacin and ciprofloxacin in pharmaceutical formulations

This work proposes a sequential injection analysis (SIA) system for the spectrophotometric determination of norfloxacin (NOR) and ciprofloxacin (CIP) in pharmaceutical formulations. The methodology was based on the reaction of these drugs with p-(dimethylamino)cinnamaldehyde in micellar medium, producing orange colored products (λmax = 495 nm). Beer´s law was obeyed in the concentration range from 2.75x10-5 to 3.44x10-4 mol L-1 and 3.26x10-5 to 3.54x10-4 mol L-1 for NOR and CIP, respectively and sampling rate was 25 h-1. Commercial samples were analyzed and results obtained through the proposed method were in good agreement with those obtained using the reference procedure for a 95% confidence level.

Sistema de análises em fluxo polivalente para a determinação espectrofotométrica de fármacos

A flow system based on the sandwich technique is proposed for the sequential determination of ascorbic acid, dipyrone, acetylcysteine, captopril and paracetamol. The procedure is based on the reduction of Cu(II) by the analytes followed by the spectrophotometric measurement of the complex of Cu(I) with 2,2'-biquinoline 4,4'-dicarboxylic acid. Linear responses were achieved in the µmol L-1 range, with coefficients of variation better than 1.7%. Sampling rate was estimated as 60 determinations per hour, consuming 230 µg of BQA and generating 2.5 mL of waste per determination. Results for commercial samples agreed with those obtained by procedures recommended by the American and European pharmacopeias at the 95% confidence level.

Indirect spectrophotometric method for determination of captopril using Cr(VI) and diphenylcarbazide

A spectrophotometric method for the indirect determination of captopril (CP) in pharmaceutical formulations is proposed. The proposed procedure is based on the oxidation of captopril by potassium dichromate and the determination excess oxidant on the basis of its reaction with diphenylcarbazide (DPC). Under the optimum conditions, a good linear relationship (r = 0.9997) was obtained in the range of 0.08-3.5 µg mL-1. The assay limits of detection and quantitation were 0.024 and 0.08 µg mL-1, respectively. The results obtained for captopril determination in pharmaceuticals using the proposed method and those obtained with the US Pharmacopoeia method were in good agreement at the 95% confidence level.

Registrador portátil de odorantes basado en la modulación de temperatura de un sensor mos comercial

A simple, portable and low-cost system for odor detection was developed using a single MOS commercial sensor and a microcontroller. The temperature modulation technique was implemented applying a DC signal pulse to the sensor heater by a bipolar transistor. Two odorant profiles, ethanol and acetic acid vapors, were obtained and distinguished based on their amplitude versus time responses. Response for acetic acid was not reported by the sensor manufacturer. An ethanol vapor calibration curve was also obtained. Experimental data showed a potential behavior according to the theoretical equation of the MOS sensors. Values of logK=0.457 and α=-0.213 for a 95% confidence level were obtained.

Avaliação de dispositivos de captura de imagens digitais para detecção colorimétrica em microzonas impressas

This report describes a study about the feasibility of using a conventional digital camera, a cell-phone camera, an optical microscope, and a scanner as digital image capture devices on printed microzones. An array containing nine circular zones was drawn using graphics software and printed onto transparency film by a laser printer. Due to its superior analytical performance, the scanner was chosen for the quantitative determination of Fe2+ in pharmaceutical samples. The data achieved using scanned images did not differ statistically from those attained by the reference spectrophotometric method at the confidence level of 0.05.

Determinação voltamétrica de amitriptilina em formulações farmacêuticas com eletrodo de diamante dopado com boro explorando medidas em meio ácido

A simple and reliable voltammetric method is presented for the determination of amitriptyline using a boron-doped diamond electrode in 0.1 mol L-1 sulfuric acid solution as the support electrolyte. Under optimized differential pulse voltammetry conditions (modulation time 5 ms, scan rate 70 mV s-1, and pulse amplitude 120 mV), the electrode provides linear responses to amitriptyline in the concentration range 1.05 to 92.60 µmol L-1 and at a detection limit of 0.52 µmol L-1. The proposed method was successfully applied in pharmaceutical formulations, with results similar to those obtained using UV-vis spectrophotometric method as reference (at 95% confidence level), as recommended by the Brazilian Pharmacopoeia.

AVALIAÇÃO DO RADICAL N,N-DIETIL-1,4-FENILENODIAMINO (DEPD•+) COMO SONDA ESPECTROFOTOMÉTRICA PARA DETERMINAÇÃO DA CAPACIDADE ANTIOXIDANTE EM BEBIDAS

AbstractMany well-established methods for determining the antioxidant capacities in several samples have been described in literature. However, DPPH (2,2-diphenyl-1-picrylhydrazyl) and ABTS (2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid)) are the main two methods that utilize radicals as spectrophotometric probes for analysis. Nevertheless, these methods have certain limitations because of their slower kinetics, solvent polarity effects, the hydrophilicity and lipophilicity of the compounds, chemical costs, etc. In this study, a spectrophotometric method for determining the antioxidant capacity in beverages was developed based on an exploration of the cation radical derived from DEPD. This method was based on the oxidation of aromatic amines with Fe(III) ions at pH 4.0, which leads to their corresponding purple cation radicals (DEPD•+) with λmax values at 500 and 540 nm. The addition of an antioxidant after the formation of the radical leads to a reduction in color intensity that is proportional to the antioxidant concentration in the medium. Results obtained using this method were compared with the Folin-Ciocalteau, ABTS and DPPH methods in terms of applications in wines, teas, and infusions samples. Linear correlation analysis at a 95% confidence level was employed to compare the results, which were in good agreement with a correlation coefficient of r > 0.9000. Thus, the developed method was simple, accurate, and consistent with other assays for the determination of the total amount of phenolic compounds and antioxidant capacity.

Flow injection spectrophotometric determination of adrenaline using a solid-phase reactor containing triiodide ions immobilized in an anion-exchange resin

A flow injection spectrophotometric procedure with on-line solid-phase reactor containing ion triiodide immobilized in an anion-exchange resin is proposed for the determination of adrenaline (epinephrine) in pharmaceutical products. Adrenaline is oxidized by triiodide ion immobilized in an anionic-exchange resin yielding adrenochrome which is transported by the carrier solution and detected at a wavelength of 488 nm. Adrenaline was determined in three pharmaceutical products in the 6.4 x 10-6 to 3.0 x 10-4 mol L-1 concentration range with a detection limit of 4.8 x 10-7 mol L-1. The recovery of this analyte in three samples ranged from 96.0 to 105 %. The analytical frequency was 80 determinations per hour and the RSDs were less than 1 % for adrenaline concentrations of 6.4 x 10-5 and 2.0 x 10-4 mol L-1 (n=10). A paired t-test showed that all results obtained for adrenaline in commercial formulations using the proposed flow injection procedure and a spectrophotometric batch procedure agree at the 95% confidence level.

Use of experimental design in the optimisation of a solid phase preconcentration system for Cobalt determination by GFAAS

In this work is proposed a solid phase preconcentration system of Co2+ ions and its posterior determination by GFAAS in which fractional factorial design and response surface methodology (RSM) were used for optimization of the variables associated with preconcentration system performance. The method is based on cobalt extraction as a complex Co2+-PAN (1:2) in a mini-column of polyurethane foam (PUF) impregnated with 1-(2-pyridylazo)-naphthol (PAN) followed by elution with HCl solution and its determination by GFAAS. The chemical and flow variables studied were pH, buffer concentration, eluent concentration and preconcentration and elution flow rates. Results obtained from fractional factorial design 2(5-1) showed that only the variables pH, buffer concentration and interaction (pH X buffer concentration) based on analysis of variance (ANOVA) were statistically significant at 95% confidence level. Under optimised conditions, the method provided an enrichment factor of 11.6 fold with limit of detection and quantification of 38 and 130 ng L-1, respectively, and linear range varying from 0.13 to 10 µg L-1. The precision (n = 9) assessed by relative standard deviation (RSD) was respectively 5.18 and 2.87% for 0.3 and 3.0 µg L-1 cobalt concentrations.

Spectrophotometric determination of methyldopa in pharmaceutical formulations

A new, simple, precise, rapid and low-cost spectrophotometric method for methyldopa determination in pharmaceutical preparations is described. This method is based on the complexation reaction of methyldopa with molybdate. Absorbance of the resulting yellow coloured product is measured at 410 nm. Beer's Law is obeyed in a concentration range of 50 - 200 µg ml-1 methyldopa with an excellent correlation coefficient (r = 0.9999). No interference was observed from common excipients in formulations. The results show a simple, accurate, fast and readily applied method to the determination of methyldopa in pharmaceutical products. The analytical results obtained for these products by the proposed method are in agreement with those of the Brazilian Pharmacopoeia procedure at 95% confidence level.

Determination of hydroquinone in a square wave voltammetry procedure using a graphite-polyurethane composite electrode

In order to a better characterization of a graphite-polyurethane composite intended to be used as a voltammetric sensor, the performance in a square wave voltammetric procedure was investigated. Using hydroquinone (HQ) as a probe, the electrode showed to be useful in square wave voltammetry with limit of detection of 0.28 µmol L-1, with recoveries between 99.1 and 101.5%. The results of the proposed method agreed with HPLC ones within 95% confidence level.