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Flow injection analysis using carbon film resistor electrodes for amperometric determination of ambroxol

Felix, Fabiana S.; Brett, Christopher M.A.; Angnes, Lúcio
Fonte: Universidade de Coimbra Publicador: Universidade de Coimbra
Tipo: Artigo de Revista Científica Formato: aplication/PDF
ENG
Relevância na Pesquisa
97.83535%
Flow injection analysis (FIA) using a carbon film sensor for amperometric detection was explored for ambroxol analysis in pharmaceutical formulations. The specially designed flow cell designed in the lab generated sharp and reproducible current peaks, with a wide linear dynamic range from 5 × 10-7 to 3.5 × 10-4 mol L-1, in 0.1 mol L-1 sulfuric acid electrolyte, as well as high sensitivity, 0.110 A mol-1 L cm-2 at the optimized flow rate. A detection limit of 7.6 × 10-8 mol L-1 and a sampling frequency of 50 determinations per hour were achieved, employing injected volumes of 100 [mu]L and a flow rate of 2.0 mL min-1. The repeatability, expressed as R.S.D. for successive and alternated injections of 6.0 × 10-6 and 6.0 × 10-5 mol L-1 ambroxol solutions, was 3.0 and 1.5%, respectively, without any noticeable memory effect between injections. The proposed method was applied to the analysis of ambroxol in pharmaceutical samples and the results obtained were compared with UV spectrophotometric and acid-base titrimetric methods. Good agreement between the results utilizing the three methods and the labeled values was achieved, corroborating the good performance of the proposed electrochemical methodology for ambroxol analysis.; http://www.sciencedirect.com/science/article/B6THP-4RW434G-1/1/d40a3f00a2eaccb84817b064f601d0f2

Flow injection analysis using carbon film resistor electrodes for amperometric determination of ambroxol

FELIX, Fabiana S.; BRETT, Christopher M. A.; ANGNES, Lucio
Fonte: ELSEVIER SCIENCE BV Publicador: ELSEVIER SCIENCE BV
Tipo: Artigo de Revista Científica
ENG
Relevância na Pesquisa
97.83535%
Flow injection analysis (FIA) using a carbon film sensor for amperometric detection was explored for ambroxol analysis in pharmaceutical formulations. The specially designed flow cell designed in the lab generated sharp and reproducible current peaks, with a wide linear dynamic range from 5 x 10(-7) to 3.5 x 10(-4) mol L-1, in 0.1 mol L-1 sulfuric acid electrolyte, as well as high sensitivity, 0.110 A mol(-1) L cm(-2) at the optimized flow rate. A detection limit of 7.6 x 10(-8) mol L-1 and a sampling frequency of 50 determinations per hour were achieved, employing injected volumes of 100 mu L and a flow rate of 2.0 mL min(-1). The repeatability, expressed as R.S.D. for successive and alternated injections of 6.0 x 10(-6) and 6.0 x 10(-5) mol L-1 ambroxol solutions, was 3.0 and 1.5%, respectively, without any noticeable memory effect between injections. The proposed method was applied to the analysis of ambroxol in pharmaceutical samples and the results obtained were compared with UV spectrophotometric and acid-base titrimetric methods. Good agreement between the results utilizing the three methods and the labeled values was achieved, corroborating the good performance of the proposed electrochemical methodology for ambroxol analysis. (C) 2008 Elsevier B.V. All rights reserved.

Desenvolvimento e avaliação de sistema envolvendo interface de análise por injeção em fluxo com eletroforese capilar; Design and evaluation of an automatic system for flow injection analysis capillary electrophoresis with contactless conductivity

Palgrossi, Fabiano Souza
Fonte: Biblioteca Digitais de Teses e Dissertações da USP Publicador: Biblioteca Digitais de Teses e Dissertações da USP
Tipo: Dissertação de Mestrado Formato: application/pdf
Publicado em 26/11/2002 PT
Relevância na Pesquisa
97.67902%
A combinação sinérgica da análise por injeção em fluxo com eletroforese capilar, FIA-CE, é um novo campo em rápida expansão, que se estende da simples justaposição de equipamentos (FIA-CE at-line) ao verdadeiro interfaceamento ou hifenação (FIA-CE in-line ou on-line). Tipicamente, circuitos FIA construídos nos laboratórios são interfaceados com equipamentos comerciais de eletroforese capilar providos com detecção espectrofotométrica UV-Vis, e operam sob injeção (ou melhor, transferência) eletrocinética de amostra do circuito FIA para o capilar, vez que esta é mais simples para implementar que a transferência hidrodinâmica. Um novo sistema FIA-CE que combina a detecção condutométrica sem contato elétrico, DCSC, com transferência hidrodinâmica ou eletrocinética de amostra foi projetado e construído no laboratório utilizando-se material de baixo custo, além de uma fonte de alta tensão, uma bomba peristáltica e um microcomputador. No circuito FIA, utilizou-se um único solenóide na construção de injetor multicanal com válvulas de estrangulamento de dimensões reduzidas. O DCSC foi anteriormente desenvolvido por outros componentes do grupo. A interface FIA-CE consiste de uma agulha hipodérmica de aço inoxidável conectada à saída do circuito FIA...

Desenvolvimento de sistemas de análises em fluxo por multicomutação para determinação de poluentes ambientais; Development of systems of flow injection analysis with commutation for determination of environmental pollutants

Córdova, Carlos Martín Infante
Fonte: Biblioteca Digitais de Teses e Dissertações da USP Publicador: Biblioteca Digitais de Teses e Dissertações da USP
Tipo: Tese de Doutorado Formato: application/pdf
Publicado em 23/09/2008 PT
Relevância na Pesquisa
97.94041%
O presente trabalho teve como objetivo o desenvolvimento de procedimentos analíticos baseados na análise em fluxo com multicomutação, acoplada à detecção por fluorescência, espectrofotometria com longo caminho óptico ou quimiluminescência em guias de ondas (LCW), para a determinação de poluentes ambientais. Os procedimentos desenvolvidos atendem aos requisitos de sensibilidade e limite de detecção impostos pela legislação ambiental vigente e as características analíticas encontram-se em concordância com as tendências atuais de redução do consumo de amostras e reagentes, da geração de resíduos e de custo, apresentando alta freqüência de amostragem e operação simples. Os módulos de análises desenvolvidos são compactos, podendo ser adaptados para o monitoramento in situ. Com o acoplamento da cela LCW de 100 cm de caminho óptico a sistemas de análises por injeção em fluxo e monossegmentado, para medidas por turbidimetria e espectrofotometria, foi observada significativa melhora nos limites de detecção e sensibilidade. Discrepâncias entre o aumento de sensibilidade verificado e previsto pela lei de Beer têm relação com diferenças de dispersão em celas de 1 e 100 cm. Para a determinação espectrofotométrica de paraquat...

Desenvolvimento de um sistema eletroquímico de análise por injeção em fluxo para detecção de cocaína; Development of an Electrochemical Flow Injection Analysis system for Detection of Cocaine

Oliveira, Laura Siqueira de
Fonte: Biblioteca Digitais de Teses e Dissertações da USP Publicador: Biblioteca Digitais de Teses e Dissertações da USP
Tipo: Dissertação de Mestrado Formato: application/pdf
Publicado em 17/01/2012 PT
Relevância na Pesquisa
97.77948%
O aumento nos índices de criminalidade, na maioria das vezes decorrente de atividades ligadas ao tráfico de drogas, afeta drasticamente a qualidade de vida do ser humano. A análise instrumental de entorpecentes é realizada comumente por métodos cromatográficos, oferecendo limites de detecção (LDs) em torno de 1 ng mL-1. As técnicas analíticas como voltametria, amperometria, potenciometria, dentre outras, assemelham-se às técnicas convencionais de análise, pois além de se mostrarem sensíveis para a análise de traços de substâncias orgânicas e inorgânicas, oferecem vantagens operacionais como a compreensão de mecanismos pato-fisiológicos de várias drogas, dentre elas a cocaína e seus metabólitos. Os eletrodos quimicamente modificados (EQMs) com bases de Schiff (grupos funcionais que contém uma ligação dupla carbono-nitrogênio com o átomo de nitrogênio conectado a um grupo arila ou alquila) desenvolvidos para a determinação de cocaína em amostras de interesse forense podem ser empregados em situação de análise por injeção em fluxo (FIA). Cuja metodologia consiste na inserção de uma alíquota de amostra em um fluido carregador que a transporta do ponto de injeção até a unidade de detecção. Atualmente a análise de cocaína está limitada à dosagem posterior de amostras apreendidas...

Direct determination of calcium in milk by atomic absorption spectrometry using flow-injection analysis

Petrovich, M. B.; Filho, V. R. A.; Neto, J. A. G.
Fonte: Editora Unesp Publicador: Editora Unesp
Tipo: Artigo de Revista Científica Formato: 25-30
ENG
Relevância na Pesquisa
87.64961%
Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP); Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq); Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES); Um sistema de injeção em fluxo envolvendo a adição de amostra e reagente por zonas coalescentes sincronizadas é proposto para a determinação de cálcio em leites por FAAS. Um planejamento fatorial com ponto central auxiliou na seleção dos principais parâmetros experimentais, sendo as condições ótimas estabelecidas em: solução de lantânio 2,5% (m/v), vazão do transportador 8 mL min-1, comprimento da bobina de reação 20 cm e volume de amostra injetado 250 ìL. Quatro procedimentos de preparo de amostra foram avaliados: diluição em ácido nítrico diluído e em água, decomposição em forno de microondas empregando ácidos concentrados e diluídos. O sistema de análise por injeção em fluxo desenvolvido foi aplicado na determinação de cálcio em onze amostras de leite comerciais e em dois materiais de referência padrão diluídos em água. Teores similares de cálcio foram encontrados comparando-se os resultados obtidos pelo método proposto (diluição em água) com aqueles obtidos nos digeridos. As concentrações de cálcio determinadas nos dois materiais de referência padrão foram concordantes a um nível de 95% de confiança com seus valores certificados. Recuperações entre 93% a 116% foram obtidas. O desvio padrão relativo (n = 12) foi < 5...

Use of a carbon paste electrode modified with spinel-type manganese oxide as a potentiometric sensor for lithium ions in flow injection analysis

Teixeira, MFS; Cavalheiro, ETG; Bergamini, M. F.; Moraes, F. C.; Bocchi, N.
Fonte: Wiley-Blackwell Publicador: Wiley-Blackwell
Tipo: Artigo de Revista Científica Formato: 633-639
ENG
Relevância na Pesquisa
97.85999%
A potentiometric sensor constructed from a mixture of 25% (m/m) spinel-type manganese oxide (lambda-MnO2), 50% (m/m) graphite powder and 25% (m/m) mineral oil is used for the determination of lithium ions in a flow injection analysis system. Experimental parameters, such as pH of the carrier solution, flow rate, injection sample volume, and selectivity for Li+ against other alkali and alkaline-earth ions and the response time of this sensor were investigated. The sensor response to lithium ions was linear in the concentration range 8.6 x 10(-5) - 1.0 x 10(-2) mol L-1 with a slope 78.9 +/- 0.3 mV dec(-1) over a wide pH range 7 - 10 (Tris buffer), without interference of other alkali and alkaline-earth metals. For a flow rate of 5.0 mL min(-1) and a injection sample volume of 408.6 muL, the relative standard deviation for repeated injections of a 5.0 x 10(-4) mol L-1 lithium ions was 0.3%.

Sequential spectrophotometric determination of chromium(III) and chromium(VI) using flow injection analysis

De Andrade, João Carlos; Rochat, Julio Cesar; Baccan, Nivaldo
Fonte: Universidade Estadual Paulista Publicador: Universidade Estadual Paulista
Tipo: Artigo de Revista Científica Formato: 197-199
ENG
Relevância na Pesquisa
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A flow injection analysis (FIA) procedure for the speciation of Cr(III) and Cr(VI) using the 1,5-diphenylcarbazide (DPC) method is presented. As Cr(III) does not interfere in the Cr(VI) - DPC reaction, both Cr(VI) and total chromium [after the on-line oxidation of Cr(III) by Ce(IV)] are sequentially determined. Cr(III) is obtained by difference. Under the experimental conditions described, the calibration graphs are linear up to 2 μg mh1 of Cr(VI) and 4 μg ml-1 of Cr(III). The detection limits found were 18 ng ml -1 for Cr(VI) and 55 ng ml-1 for Cr(III), at a signal to noise ratio of 3. The common interfering elements in the Cr(VI) - DPC reaction were investigated under dynamic FIA conditions. The FIA method was also compared with the conventional spectrophotometric procedure.

Rapid determination of zinc in foods by flow injection analysis with flame AAS using gradient calibration method

Anzano, Jesús M.; Heinemann, Riana J. B.; Mir, José Ma.
Fonte: Universidade Estadual Paulista Publicador: Universidade Estadual Paulista
Tipo: Artigo de Revista Científica Formato: 221-225
ENG
Relevância na Pesquisa
98.02934%
A calibration method was developed using flow injection analysis (FI) with a Gradient Calibration Method (GCM). The method allows the rapid determination of zinc In foods (approximately 30 min) after treatment with concentrated sulphuric acid and 30% hydrogen peroxide, and analysis with flame atomic absorption spectrometry (FAAS). The method provides analytical results with a relative standard deviation of about 2% and requires less time than by conventional FI calibration. The electronic selection of different segments along the gradient and monitoring of the technique covers wide concentration ranges while maintaining the inherent high precision of flow injection analysis. Concentrations, flow rates, and flow times of the reagents were optimized in order to obtain best accuracy and precision. Flow rates of 10 mL/min were selected for zinc. In addition, the system enables electronic dilution and calibration where a multipoint curve can be constructed using a single sample injection.

Flow-through solid-phase based optical sensor for the multisyringe flow injection trace determination of orthophosphate in waters with chemiluminescence detection

Morais, Inês P.A.; Miró, Manuel; Manera, Matias; Estela, José Manuel; Cerdà, Víctor; Souto, M. Renata S.; Rangel, António O.S.S.
Fonte: Elsevier Publicador: Elsevier
Tipo: Artigo de Revista Científica
Publicado em //2004 ENG
Relevância na Pesquisa
87.92247%
In this work, a novel flow-through solid-phase based chemiluminescence (CL) optical sensor is described for the trace determination of orthophosphate in waters exploiting the multisyringe flow injection analysis (MSFIA) concept with multicommutation. The proposed time-based injection flow system relies upon the in-line derivatisation of the analyte with ammonium molybdate in the presence of vanadate, and the transient immobilisation of the resulting heteropolyacid in a N-vinylpyrrolidone/divinylbenzene copolymer packed spiral shape flow-through cell located in front of the window of a photomultiplier tube. The simultaneous injection of well-defined slugs of luminol in alkaline medium and methanol solution towards the packed reactor is afterwards performed by proper switching of the solenoid valves. Then, the light emission from the luminol oxidation by the oxidant species retained onto the sorbent material is readily detected. At the same time, the generated molybdenum-blue compound is eluted by the minute amount of injected methanol, rendering the system prepared for a new measuring cycle. Therefore, the devised sensor enables the integration of the solid-phase CL reaction with elution and detection of the emitted light without the typical drawbacks of the molybdenum-blue based spectrophotometric procedures regarding the excess of molybdate anion...

Enzymatic determination of L(-)malic and L(+)lactic acids in wine by flow injection analysis

Lima, José L. F. C.; Rangel, António O. S. S
Fonte: American Society for Enology and Viticulture Publicador: American Society for Enology and Viticulture
Tipo: Artigo de Revista Científica
Publicado em //1992 ENG
Relevância na Pesquisa
97.75175%
The enzymatic determination of L(-)malic and L(+)lactic acids in several types of wines by flow injection analysis (FIA) with spectrophotometric detection is described. This flow injection system, which incorporates a dialysis unit for adjusting the composition of the injected solutions to the requirements of the measuring system, enables determinations of these two organic acids without the need for any prior treatment of the wine samples, with a concentration interval of between 0.02 and 4 g/L, and a sampling rate of approximately 20 determinations per hour. The results obtained with this FIA method for various types of Portuguese wines are in good agreement with those of the batch method which uses the same enzymatic technique and are quite precise as they present a coefficient of variation below 2.5%.

Multi-syringe flow injection system for the determination of available phosphorus in soil samples

Almeida, M. Inês G. S.; Segundo, Marcela A.; Lima, José L. F. C.; Rangel, António O. S. S.
Fonte: Taylor & Francis Publicador: Taylor & Francis
Tipo: Artigo de Revista Científica
Publicado em //2005 ENG
Relevância na Pesquisa
87.64961%
Considering the importance of monitoring the levels of nutrients present in soils and their availability to plants, an automatic methodology is proposed based on multi-syringe flow injection analysis (MSFIA) for the spectrophotometric determination of available phosphorus in soil extracts. This fully computerized flow technique allowed the development of a flow network where sample and reagents were intercalated and sent further towards the detection system. The colorimetric determination was based on the molybdenum blue method with ascorbic acid as reducing reagent and the Egner–Riehm method was applied to extract phosphorus from soil samples. A linear calibration curve was obtained between 0.75 and 15.0mgL-1. A determination frequency of 15 h-1 was achieved, with good repeatability for 12 consecutive injections of soil extracts (RSD<1.7%). The results obtained from 12 soil samples were statistically comparable to those attained by the usual batch method.

Direct determination of calcium in milk by atomic absorption spectrometry using flow-injection analysis

Petrovich,M. B.; Filho,V. R. A.; Neto,J. A. G.
Fonte: Fundação Editora da Universidade Estadual Paulista Júlio de Mesquita Filho - UNESP Publicador: Fundação Editora da Universidade Estadual Paulista Júlio de Mesquita Filho - UNESP
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/01/2007 EN
Relevância na Pesquisa
87.64961%
A flow-injection system with sample and reagent addition by the synchronous merging zones approach for calcium determination in milk by flame AAS is proposed. Main parameters were optimized using a factorial design with central point. The optimum conditions were 2.5% (m/v) for La concentration, 8 mL min-1 for the carrier flow-rate, 20 cm for coiled reactor and 250 ìL for sample volume. Different sample preparation procedures were evaluated such as dilution in water or acid and microwave-assisted decomposition using concentrated or diluted acids. The optimized flow system was applied to determine Ca in eleven commercial milk samples and two standard reference materials diluted in water. Similar calcium levels were encountered comparing the results obtained by the proposed method (dilution in water) with those obtained using microwave-oven digestion. Results obtained in two standard reference materials were in agreement at 95% confidence level with those certified. Recoveries of spiked samples were in the 93% - 116% range. Relative standard deviation (n = 12) was < 5.4% and the sample throughput was 150 measurements per hour, corresponding to a consumption of 250 µL of sample and 6.25 mg La per determination.

Determination of boron in natural water and products derived from grape using an automated flow injection analysis system with piezoelectric detection

Jesus,Dosil P. de; Saito,Renata M.; Lago,Claudimir L. do
Fonte: Sociedade Brasileira de Química Publicador: Sociedade Brasileira de Química
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/10/2004 EN
Relevância na Pesquisa
97.59197%
An automated flow injection analysis system with piezoelectric detection is proposed as a sensitive and selective method for boron. The detector is an electrode-separated piezoelectric quartz crystal coated with N-methyl-D-glucamine-modified poly(epichlorohydrin). The film ability to retain boron allows the adjustment of the linear dynamic range and the sensitivity by varying the injected sample volume. In the present work, the sample volumes were varied from 0.5 to 5.0 mL. Among several ionic species, germanate is the only one that can interfere in the method. Nevertheless, it can be eliminated by addition of sulfide to the sample. The method was successfully applied to the determination of boron concentration in samples of natural water (from 1.71 to 309 µL-1) and products derived from grape juice (from 2.06 to 6.21 mg L-1). A pretreatment with hydrogen peroxide in alkaline medium was required due to the great amount of sugars in the grape products.

Determination of sildenafil citrate (Viagra®) in various pharmaceutical formulations by flow injection analysis with multiple pulse amperometric detection

Lopes Júnior,Antônio Carlos V.; Luz,Rita de Cássia Silva; Damos,Flávio S.; Santos,Alexandre S. dos; Franco,Diego L.; Santos,Wallans T. Pio dos
Fonte: Sociedade Brasileira de Química Publicador: Sociedade Brasileira de Química
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/10/2012 EN
Relevância na Pesquisa
97.59197%
This work presents a simple, fast and low-cost method for determining sildenafil citrate (SC) in Viagra® and in similar, generic and manipulated pharmaceutical formulations using flow injection analysis (FIA) with multiple pulse amperometric detection. The method consists on the application of three sequential potential pulses as a function of time. SC is detected at 1.6 and 1.9 V by two different irreversible oxidation processes. The third potential pulse (1.0 V) is applied for the regeneration (cleaning) of the surface of the boron-doped electrode. The limit of detection on an order of 10 nmol L-1 was reached with a relative standard deviation of less than 0.2% (n = 10) for 4.5 X 10-5 mol L-1 CS. The analytical frequency was calculated in 86 injections per hour. The addition recovery studies in all the samples were approximately 100% and the results were validated by chromatographic methods.

Estudos para a determinação amperométrica de nitrofosforados totais em águas em sistema de análise por injeção em fluxo; Studies for the amperometric determination of total nitrophosphates in waters in flow injection analysis

Santos, Wallans Torres Pio dos
Fonte: Universidade Federal de Uberlândia Publicador: Universidade Federal de Uberlândia
Tipo: Dissertação
POR
Relevância na Pesquisa
97.78039%
No presente trabalho investigou-se uma metodologia de determinação eletroquímica de Paration baseada na detecção amperométrica de múltiplos pulsos em sistema de análise por injeção em fluxo (FIA). Um sistema de propulsão isento de pulsação e um detector eletroquímico para sistemas de análise em fluxo foram construídos e investigados para esta determinação. Estudos do comportamento eletroquímico do Paration sobre eletrodos de carbono foram investigados em função do pH e do tipo de eletrólito suporte. Eletrodo de carbono vítreo e ácido cítrico 0,1 mol L-1 forneceram as condições experimentais mais favoráveis para a detecção amperométrica de Paration. Os estudos da detecção amperométrica de múltiplos pulsos, no modo gerador-coletor, sob condições de análise em fluxo, indicaram que este modo de detecção aumenta a sensibilidade e a seletividade da determinação eletroquímica do Paration. Sinais amperométricos mais estáveis e de maior sensibilidade foram obtidos quando pulsos de potencial eram aplicados na seqüência, -0,5 V, +0,4 V e -0,1 V, durante 30 ms cada. A aplicação destes pulsos de potenciais envolveu os seguintes processos de eletrodo, respectivamente: redução de RNO2 a RNHOH, oxidação de RNHOH a RNO e redução de RNO a RNHOH. O desvio padrão relativo dos sinais amperométricos obtidos em -0...

Investigations in flow injection analysis (FIA): conventional FIA determination of chloride in water; sequential injection (SI)-FIA determination of mercury in water

Cirello-Egamino, Joanne.
Fonte: Brock University Publicador: Brock University
Tipo: Electronic Thesis or Dissertation
ENG
Relevância na Pesquisa
97.84702%
Flow injection analysis (FIA) was applied to the determination of both chloride ion and mercury in water. Conventional FIA was employed for the chloride study. Investigations of the Fe3 +/Hg(SCN)2/CI-,450 nm spectrophotometric system for chloride determination led to the discovery of an absorbance in the 250-260 nm region when Hg(SCN)2 and CI- are combined in solution, in the absence of iron(III). Employing an in-house FIA system, absorbance observed at 254 nm exhibited a linear relation from essentially 0 - 2000 Jlg ml- 1 injected chloride. This linear range spanning three orders of magnitude is superior to the Fe3+/Hg(SCN)2/CI- system currently employed by laboratories worldwide. The detection limit obtainable with the proposed method was determin~d to be 0.16 Jlg ml- 1 and the relative standard deviation was determined to be 3.5 % over the concentration range of 0-200 Jig ml- 1. Other halogen ions were found to interfere with chloride determination at 254 nm whereas cations did not interfere. This system was successfully applied to the determination of chloride ion in laboratory water. Sequential injection (SI)-FIA was employed for mercury determination in water with the PSA Galahad mercury amalgamation, and Merlin mercury fluorescence detection systems. Initial mercury in air determinations involved injections of mercury saturated air directly into the Galahad whereas mercury in water determinations involved solution delivery via peristaltic pump to a gas/liquid separator...

Flow injection analysis of vancomycin

Vila,M. M. D. C.; Salomão,A. A.; Tubino,M.
Fonte: Fundação Editora da Universidade Estadual Paulista Júlio de Mesquita Filho - UNESP Publicador: Fundação Editora da Universidade Estadual Paulista Júlio de Mesquita Filho - UNESP
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/01/2008 EN
Relevância na Pesquisa
87.75175%
A flow injection method for the quantitative analysis of vancomycin hydrochloride, C66H75Cl2N9O24.HCl (HVCM), based on the reaction with copper (II) ions, is presented. HVCM forms a lilac-blue complex with copper ions at pH≅4.5 in aqueous solutions, with maximum absorption at 555 nm. The detection limit was estimated to be about 8.5×10-5 mol L-1; the quantitation limit is about 2.5×10-4 mol L-1 and about 30 determinations can be performed in an hour. The accuracy of the method was tested through recovery procedures in presence of four different excipients, in the proportion 1:1 w/w. The results were compared with those obtained with the batch spectrophotometric and with the HPLC methods. Statistical comparison was done using the Student's procedure. Complete agreement was found at a 0.95 significance level between the proposed flow injection and the batch spectrophotometric methods, which present similar precision (RSD: 2.1 % vs. 1.9%).

Flow injection analysis with amperometric detection for morpholine determination in corrosion inhibitors

Oliveira,Sanair M. de; Siguemura,Angelo; Lima,Hugo O.; Souza,Flávia C. de; Magalhães,Alvaro A. O.; Toledo,Roberta M.; D'Elia,Eliane
Fonte: Sociedade Brasileira de Química Publicador: Sociedade Brasileira de Química
Tipo: Artigo de Revista Científica Formato: text/html
Publicado em 01/08/2014 EN
Relevância na Pesquisa
97.59197%
In this study, an electrochemical method is proposed using flow injection analysis and amperometric detection with screen-printed carbon electrodes for morpholine determination to monitor the quality of morpholine-based commercial inhibitors and the residual concentration of inhibitors that control internal corrosion in oil industry pipelines. The amperometric method resulted in a strong linear correlation coefficient (r = 0.9941) with a linear response over a concentration range of 20-120 mg L-1, a limit of detection of 10 mg L-1 and a limit of quantification of 30 mg L-1. In addition, the method has been shown to be precise, linear and homoscedastic. The recovery for the amperometric method was 100 ± 6%, and the recovery for the real condensate sample was 99 ± 2%. Thus, the proposed method is promising for analysing morpholine-based commercial inhibitors in oil industry pipelines with simple and low-cost methodologies compared with ion chromatography techniques.

Use of poly(ester-sulfonic acid) film-coated electrodes as amperometric detectors in flow injection analysis

Gennett, Thomas; Rusin, W.; Gier, L.
Fonte: Elsevier: Talanta Publicador: Elsevier: Talanta
Tipo: Abstract Formato: 37365 bytes; application/pdf
EN_US
Relevância na Pesquisa
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Within the past several years significant advances have been made towards the development and incorporation of chemically modified electrodes as selective detectors for high performance liquid chromatography and flow injection analysis. In many cases the chemically modified electrode systems closely approach the ''ideal'' detector specifications of chemical and mechanical stability along with a significant linear response region. This paper will discuss the characterization and incorporation of ionomeric poly(ester-sulfonic acid) coated electrodes as nonaqueous electrochemical detectors. The orientation of the electrodes in the detector system as well as the increased sensitivity levels to 10-10 g ml-1 for cationic species and 10-9 g ml-1 for neutral species will be presented. Also the applicability of the ionomer coated electrodes as nonelectrolyte detectors achieved a reproducible response with detection limits to 10-6 g ml-1. Overall this system performed as well as, or better than, more specialized and expensive thin layer electrochemical detectors.; The authors wish to acknowledge the financial support of the Eastman Kodak Company Outreach Grant; The Research Corporation, Cottrell Grant; and the National Science Foundation, Research Experiences for Undergraduates Program.