968 resultados para Matrix effect


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Enzyme-Linked Immunosorbent Assay (ELISA) has been evaluated by analyzing rich-humic water samples from tropical rivers. The samples were spiked with atrazine at ppb level Different pHs (4 to 9) and humic concentrations (2.5 to 40 mg L-1) were investigated. The assay performance showed a strong dependence on the pH values and amount of humic matter at low atrazine concentration. From all the conditions studied the low pH (pH 4) and high humic substances concentrations (40 mg L-1) showed the greatest influence. The IC50 value to control sample (no humic) diminished from 0.28 nmol L-1 to 0.64 nmol L-1 to humic acid solution. This effect is specially noted for the humic acid fractions, since fulvic acid fractions showed no significant change on the immunoassay results. Additionally, it has been demonstrated that at basic pH the matrix effect produced by the natural Brazilian water sample containing humic substances even at 40 mg L-1 disappears. Therefore, the ELISA method used to determine atrazine, can be employed to determine this pesticide in water samples containing humic substances without prior preparation.

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Immunochemical methods have increased considerably in the past years, and many examples of small and large scale studies have demonstrated the reliability of the immunotechniques for control and monitoring gf contaminant residues in different kinds of samples. Application of the immunoassay (IA) methods in pesticide residue control is an area with enormous potential for growth. The most extensively studied IA is the enzyme-linked absorbent assay (ELISA), but several other approaches, that include radioimmunoassay and immunoaffinity chromatography, have been also developed recently. In comparison with classical analytical methods, IA methods offer the possibility of highly sensitive, relatively vapid, and cost-effective measurements. This paper introduces the general IAs used until now, focusing on their use in pesticide analysis, and discussing briefly the effects of interferences from solvent residues or matrix components on the IA performance. Numerous immunochemical methods commonly used for pesticide determination in different samples such as food, crop and environmental samples are presented.

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Enzyme-linked immunosorbent assays (ELISAs) are the most extensively studied types of immunoassay and their application in pesticide residue monitoring is an area with enormous potential for growth. In comparison with classical analytical methods, ELISA methods offer the possibility of highly sensitive, relatively rapid, and cost-effective measurements. This review introduces the general ELISA formats used, focusing on their use in pesticide analysis. Identifying and studying the effects of interferences in immunoassays is an active area of research and we discuss the matrix effects observed in several studies involving e.g. food, crop and environmental samples. The procedures to eliminate the matrix interferences are briefly discussed. (C) 1998 Elsevier B.V. B.V.

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A competitive enzyme-linked immunosorbent assay (ELISA) method for carbaryl quantitation in crop extracts was validated by liquid chromatography (LC) with diode array detection (DAD). For this purpose, six crops (banana, carrot, green bean, orange, peach and potato) were chosen for recovery and reproducibility studies. The general sample preparation included extraction with methanol followed by liquid-liquid partitioning and clean-up on Celite-charcoal adsorbent column of the vegetable extracts. ELISA samples consisted of a diluted LC extract in assay phosphate buffer (pH 7.5). The potential effect of methanol in these samples was evaluated. It was observed that a maximum content of 10% methanol present in the assay buffer could be tolerated without expressive losses in the ELISA performance. Under these conditions, a IC50 similar to 1.48 mu g l(-1) was obtained. A minimum matrix effect with a 1:50 dilution of the methanolic extracts in assay buffer was noticed, except for green bean samples that inhibited completely the assay. For the vegetable extracts, the ELISA sensitivities varied from 3.9 to 5.7 mu g l(-1), and good recoveries (82-96%) with R.S.D.s ranging from 5.7 to 12.1% were found. An excellent correlation between the LC-DAD and ELISA techniques was obtained. The confirmation of the carbaryl in less concentrated samples was achieved by LC-mass spectrometry interfaced with atmospheric pressure chemical ionisation. The [M + H](+)= 202 and [M + H-57](+)=145 ions, equivalent to the protonated molecular and l-naphthol ions, respectively, were used to carbaryl identification in these samples. (C) 1998 Elsevier B.V. B.V. All rights reserved.

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A rapid and efficient method is described for the determination of thiabendazole and imazalil residues in lemons (peel and pulp). The procedure is based on the extraction with an hexane:ethyl acetate mixture (1:1, v/v) and gas chromatographic analysis using thermionic specific detection (TSD). The possibility of matrix effect was also studied. Mean recoveries from 8 replicates of fortified samples ranged from 79% to 109%, with relative standard deviation values between 2.4% to 12.8%. The detection and quantification limits of the method were 0.2 mg kg-1 and 0.5 mg kg-1, respectively.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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ABSTRACT: In Guajará bay, mouth of the Amazon River, is located the capital of Pará state (Belém) and its metropolitan area. Exists in this area an intense boat traffic, as well as transportation and sale of fuels in floating docks and activities related to the storage and transportation of oil in Miramar Petrochemical Terminal (TEMIR). Small spills and discharges of oil in water can serve as sources of pollution by polycyclic aromatic hydrocarbons (PAHs). PAHs are organic compounds generated by incomplete combustion of organic matter (OM) and are among the contaminants of most interest in environmental studies due to their mutagenic and carcinogenic potential. One way to detect and evaluate the impact of PAHs in an environment is using biomonitors, however the qualitative and quantitative analysis in sediments are most widely used. This study aimed to evaluate, by Gas Chromatography/Mass Spectrometry (GC/MS), the 16 PAHs considered as priority by the Environmental Protection Agency of the United States in sediments and benthic organisms (Namalicastys abiuma) of TEMIR. Field expeditions were carried out in December 2012, March, May and June 2013 representing the dried, wet (two samples) and dried seasons successively. Fine sediments levels dominated in both sampling periods and the %Fines in Guajará bays has a direct relationship to the %OM. In relation to the 16 PAHs studied, 10 of them were detected in the wet season sediments samples and 8 in the dried season. Even with a low diversity of aromatic compounds, sediment samples of the dried season presented greater ΣHPAs (1.351,43 ng g-1) than the sediments of the wet season (263,99 ng g-1), which can be related to the increased hydrodynamic in Guajará bay this last period. Correlation analysis indicated that ΣHPAs not seem to be influenced by %Fine and %OM. Benzo(a)pyrene accounted for 87% of ΣHPAs during the wet season, the other PAHs showed percentage ≤ 3%. During the other period stood out: pyrene (18% of ΣHPAs) fluoranthene (16%), the chrysene, benzo(b)fluoranthene (15%) and benzo(a)pyrene (11%). The use of the geochemical reason to interpret likely sources of PAHs indicated that there is a predominance of aromatics from pyrolytic origin in TEMIR. The activities that may be responsible for the PAHs levels observed in sediments and benthic organisms in TEMIR are the discharge of untreated domestic sewage and the emissions of particulates from cars and small/medium boats. The ΣHPAs seems to influence the density of polychaetes because a reduction of about 50% in the number of organisms was observed during the dry season when there was the greater amount of ΣHPAs in their body structure. Among the 16 PAHs studied, 11 were detected in the polychaetes during the dry season (ΣHPAsMED = 848,71 ng g-1) and 10 in the wet season (ΣHPAsMED = 141,85 ng g-1). Were highlighted during the dried season: indeno(1,2,3-c,d)pyrene (47%) and pyrene (23%). While in the wet season: pyrene (23%), chrysene (17%), fluorene (17%) and fluoranthene (13%). The %Rec obtained was >>100% indicating a matrix effect and reducing the quantitative accuracy of results. The use of the polychaete N. abiuma as biomonitor of pollution by PAHs in estuaries not seem to be effective when the sample period is limited, because collecting it requires a great effort to obtain a small amount of mass and it still results in a matrix effect in the chromatographic analysis (method %Rec >> 100%) that may not be corrected due to the restricted availability of sample mass. Studies with a larger number of samples, enabling depth statistical analysis, and covering other collection points in Guajará bay are required to prove mathematically that has been stated in this dissertation.

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Pós-graduação em Química - IQ

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

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Pós-graduação em Alimentos e Nutrição - FCFAR

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)