RESUMO
RESUMO A pesquisa descreve a reação espectrofotométrica do complexo Cu(II)-PAN (1-(2-piridilazo)-2-naftol) e determina a concentração de cobre (II) em aguardente de mandioca (Tiquira). Para isso, dimensionamos a reação para os estudos de absorção do complexo, pH, estabilidade, proporção estequiométrica, interferentes, correlação e recuperação. Após essa etapa, determinamos a concentração de cobre(II) em cinco amostras de bebidas destiladas artesanalmente de cinco municípios do Estado do Maranhão. O resultados mostram que o complexo absorve em 548 nm em pH 6, é estável em um tempo de 7 horas em proporções estequiométrica mínima de 1:1 do ligante e metal, possui limite de detecção em 3,3 X 10-2 mg L-1, faixa de linearidade de 1 X 10-6 a 1 X 10-5 mol L-1, correlação (R2= 0,9990), desvio padrão=0,0035 e recuperação em 104,54 ± 7,01 e os principais íons interferentes são o ferro (III) e o cobalto (II). Na aguardente, constatamos que o teor de cobre está acima do permitido pela legislação brasileira.
SUMMARY The search describes the spectrophotometric reaction of the Cu (II)-PAN (1-(2-pyridilazo) -2-naphthol) complex and determines the concentration of copper (II) in manioc spirit (Tiquira). For this, we dimensioned the reaction for the studies of complex absorption, pH, stability, stoichiometric ratio, interferences, correlation, and recovery. After this step, we determined the concentration of copper (II) in five samples of beverages distilled artisanal from five municipalities of the State of Maranhão. The results show that the complex absorbs at 548 nm at pH 6, is stable at a time of 7 hours in minimum 1:1 stoichiometric proportions of the binder and metal, has a detection limit in 3.3 X 10-2 mg L-1, range (R2= 0.9990), standard deviation= 0.0035 and recovery at 104.54 ± 7.0, and the main interfering ions are iron (III) and cobalt (II). In the brandy, we find that the copper content is above that allowed by Brazilian legislation.
RESUMO
RESUMO Este trabalho descreveu e comparou quatro estudos entre si que utilizaram métodos automáticos em fluxo com detecção espectrofotométrica e a reação de oxidação do diclofenaco para determinar diclofenaco em formulações farmacêuticas e fluidos corporais. Para isso, utilizamos os seguintes artigos: Versatility of a multicommuted flow system in the spectrometric determination of three analytes, Sequential injection spectrophotometric method for the assay of anti-inflammatory diclofenac sodium in pharmaceutical preparations, Screening of conditions controlling spectrophotometric sequential injection analysis e Sequential injection spectrophotometric determination of diclofenac in urine and pharmaceutical formulations e detalhamos as metodologias empregadas, os resultados, conclusões obtidas e comparamos entre eles os limites de detecção, desvio padrão relativo e a frequência analítica. Os resultados mostraram diferenças significativas entre métodos empregados e a utilização do Sistema automático do tipo Análise por Injeção Sequencial, apesar deste possuir menor frequência analítica.
SUMMARY This study described and compared four studies that used automatic flow methods with spectrophotometric detection and the oxidation reaction of diclofenac to determine diclofenac in pharmaceutical formulations and body fluids. For this, the following articles were used: Versatility of a multicommuted flow system in the spectrometric determination of three analytes, Sequential injection spectrophotometric method for the assay of anti-inflammatory diclofenac sodium in pharmaceutical preparations, Screening of conditions controlling spectrophotometric sequential injection analysis and Sequential injection spectrophotometric determination of diclofenac in urine and pharmaceutical formulations and we detail the methodologies used, the results, the conclusions obtained and compare the limits of detection, relative standard deviation and analytical frequency. The results showed significant differences between the employed methods and the use of the Automatic System of the Sequential Injection Analysis type, although this one has a lower analytical frequency.
RESUMO
RESUMO Este trabalho avalia as propriedades-físico químicas do óleo essencial dos botões florais seco do cravo-da-índia (Syzygium aromaticum) que são encontradas no Municipio de São Luís, Maranhão. Extraiu-se quantitativamente o óleo essencial por hidrodestilação. Determinaram-se as propriedades físico-químicas do óleo essencial (densidade, índice de refração, solubilidade, cor e aparência) e atividade citotóxica frente às larvas da Artemia salina. Caracterizou-se analiticamente o óleo por cromatografia gasosa acoplada a espectrómetro de massas (CG-EM). Os resul tados mostram que o melhor tempo e o rendimento do óleo foram correspondente mente 4 horas e 4,33 % de massa por volume. A partir disso foi possível identificar 5 componentes, sendo a presença majoritária do eugenol que logo foi confirmada pelas técnicas espectroscópica. Na identificação do componente majoritário e dos demais componentes, bem como suas quantificações, as técnicas foram precisas e os métodos eficientes, proporcionando um bom desempenho analítico nas determinações.
Summary This work evaluates the physical-chemical properties of the essential oil of the dry floral buds of clove (Syzygium aromaticum) that are found in the Municipality of Saint Louis, Maranhão. The essential oil was quantitatively extracted by hydrodistil lation. The physicochemical properties of the essential oil (density, refractive index, solubility, color and appearance) and cytotoxic activity against larvae of Artemia salina were determined. The oil was analytically characterized by gas chromatog raphy coupled to mass spectrometer (GC-MS). The results show that the best time and yield of the oil were correspondingly 4 hours and 4.33% mass per volume. From this, it was possible to identify five components, being the major presence of eugenol that soon was confirmed by the spectroscopic techniques. In the identification of the major component and the other components, as well as their quantifications, the techniques were precise and the methods efficient, providing a good analytical performance in the determinations.
RESUMO
A digital image-based flame emission spectrometric (DIB-FES) method for the quantitative chemical analysis is proposed here for the first time. The DIB-FES method employs a webcam to capture the digital images which are associated to a radiation emitted by the analyte into an air-butane flame. Since the detection by webcam is based on the RGB (red-green-blue) colour system, a novel mathematical model was developed in order to build DIB-FES analytical curves and estimate figures of merit for the proposed method. In this approach, each image is retrieved in the three R, G and B individual components and their values were used to define a position vector in RGB three-dimensional space. The norm of this vector is then adopted as the RGB-based value (analytical response) and it has revealed to be linearly related to the analyte concentration. The feasibility of the DIB-FES method is illustrated in three applications involving the determination of lithium, sodium and calcium in anti-depressive drug, physiological serum and water, respectively. In comparison with the traditional flame emission spectrometry (trad-FES), no statistic difference has been observed between the results by applying the paired t-test at the 95% confidence level. However, the DIB-FES method has offered the largest sensitivities and precision, as well as the smallest limits of detection and quantification for the three analytes. These advantageous characteristics are attributed to the trivariate nature of the detection by webcam.
Assuntos
Metais/análise , Espectrofotometria Atômica/métodos , Cálcio/análise , Cálcio/sangue , Estudos de Viabilidade , Humanos , Processamento de Imagem Assistida por Computador , Lítio/análise , Lítio/sangue , Metais/sangue , Preparações Farmacêuticas/análise , Sódio/análise , Sódio/sangueRESUMO
A portable, microcontrolled and low-cost spectrophotometer (MLCS) is proposed. The instrument combines the use of a compact disc (CD) media as diffraction grid and white light-emitting diode (LED) as radiation source. Moreover, it employs a phototransistor with spectral sensitivity in visible region as phototransductor, as well as a programmable interrupt controller (PIC) microcontroller as control unit. The proposed instrument was successfully applied to determination of food colorants (tartrazine, sunset yellow, brilliant blue and allura red) in five synthetics samples and Fe(2+) in six samples of restorative oral solutions. For comparison purpose, two commercial spectrophotometers (HP and Micronal) were employed. The application of the t-paired test at the 95% confidence level revealed that there are not significant differences between the concentration values estimated by the three instruments. Furthermore, a good precision in the analyte concentrations was obtained by using MLCS. The overall relative standard deviation (R.S.D.) of each analyte was smaller than 1.0%. Therefore, the proposed instrument offers an economically viable alternative for spectrophotometric chemical analysis in small routine, research and/or teaching laboratories, because its components are inexpensive and of easy acquisition.