Determinação da composição química do molusco Anadara notabilis encontrado em Galinhos no Rio Grande do Norte

Given the large existing biodiversity in the Brazilian coast, where many species are still little known, even under the nutritional aspect, and considering that bivalve molluscs are constituted by a natural resource of well accepted by the population, chose the bivalve Anadara notabilis, it was not found in the literature any nutritional or toxicological information about it and because its size is much larger than other species of mollusks commonly found in this region. Were studied moisture, ash, protein, macro and micro minerals, and metal ions of toxicological significance. All analytical determinations followed the standards of the Institute Adolfo Lutz. The protein determination was performed by the Kjeldahl method. All metal ions were determined by optical emission spectroscopy with inductively coupled plasma (ICP-OES) method described by USEPA 6010C. The results showed that Anadara notabilis can be introduced into food for human beings, in view of its mineral wealth. Noteworthy among the macronutrients phosphorus and magnesium showed that their values in mg / kg 918.7 and 586.7. With regard to micronutrients stand out with this iron 586.7 mg / kg and zinc with 12.31 mg / kg. Was not found high content of metal contaminants to this mollusc, which would prevent their use, only this chromium 0.7 mg / kg above the value established by Brazilian legislation. The results will certainly be very useful in future studies of nutrition and to build a table of chemical composition of Brazilian foods

Monitoramento das águas da bacia hidrográfica pirangi pela determinação dos índices de qualidade da água-iqa e índice de toxidez-it

The problems of water supply in Northeast Brazil are severe and require more focused studies. This work was intended to assess water quality in the watershed Pirangi, located in the Northeastern state of the newborn using the Water Quality Index, AQI associated with the Index of Toxicity-IT. The data presented in this study were collected in November 2008, June 2009 and March 2010 at eight sampling stations distributed throughout the basin. The study covered nine parameters, based on guidelines established by CETESB, and seven members of Metal Toxicity index-IT. These waters are framed in the classification between GOOD and BAD showing AQI 41.34 minimum and a maximum of 76.23. Virtually all seven metals analyzed were below the detection limits of ICP-OES giving IT a water equal to one when they are absent and 0 when there are levels of trace metals

Avaliação da influência da matéria orgânica, na determinação quantitativa de metais em amostras de sedimento, por espectrometria de absorção atômica e análise de metais traços por fluorescência de raios-X

The proposal of this work is to evaluate the influence of the organic matter on the results of the analyses of the metals (Zn, Pb, Al, Cu, Cr, Fe, Cd e Ni) for Atomic Absorption Spectrometry (AAS), so much in the extraction stage as in the reading using for that the chemometrics. They were used for this study sample of bottom sediment collected in river Jundiaí in the vicinity of the city of Macaíba-RN, commercial humus and water of the station of treatment of sewer of UFRN. Through the analyses accomplished by EAA it was verified that the interference of the organic matter happens in the extraction stage and not in the reading. With relationship to the technique of X Ray Fluorescence Spectrometry (XRFS), the present work has as intended to evaluate the viability of this technique for quantitative analysis of trace metals (Cr, Ni, Cu, Zn, Rb, Sr and Pb) in having leached obtained starting from the extraction with acqua regia for an aqueous solution. The used samples constitute the fine fraction (<0.063 mm) of sediments of swamp of the river Jundiaí. The preparation of tablets pressed starting from the dry residue of those leached it allowed your analysis in the solid form. This preliminary study shows that, in the case of the digestion chemistry partially of the fine fractions of bottom sediments used for environmental studies, the technique of applied EFRX to the analysis of dry residues starting from having leached with acqua regia, compared her it analyzes of the leached with ICP-OES, it presents relative mistakes for Cu, Pb, Sr and Zn below 10%

Determinação do teor de cálcio através da termogravimetria, em medicamentos utilizados no tratamento da osteoporose: um estudo comparativo

The present study utilized the thermogravimetry (TG) and optical emission spectroscopy with inductively coupled plasma - ICP / OES to determine the calcium content in tablets of carbonate, citrate and calcium lactate used in the treatment of osteoporosis. The samples were characterized by IR, SEM, TG / DTG, DTA, DSC and XRD. The thermal analysis evaluated the thermal stability and physical-chemical events and showed that the excipients influence the decomposition of active ingredients. The results of thermogravimetry indicated that the decomposition temperature of the active CaCO3 (T = 630.2 °C) is lower compared to that obtained in samples of the tablets (633.4 to 655.2 °C) except for sample AM 2 (Ti = 613.8 oC). In 500.0 °C in the samples of citrate and calcium lactate, as well as their respective active principles had already been formed calcium carbonate. The use of N2 atmosphere resulted in shifting the initial and final temperature related to the decomposition of CaCO3. In the DTA and DSC curves were observed endo and exothermic events for the samples of tablets and active ingredients studied. The infrared spectra identified the main functional groups in all samples of active ingredients, excipients and tablets studied, such as symmetric and asymmetric stretches of the groups OH, CH, C = O. Analysis by X-ray diffraction showed that all samples are crystalline and that the final residue showed peaks indicative of the presence of calcium hydroxide by the reaction of calcium oxide with moisture of the air. Although the samples AM 1, AM 2, AM 3 and AM 6 in their formulations have TiO2 and SiO2 peaks were not observed in X-ray diffractograms of these compounds. The results obtained by TGA to determine the calcium content of the drugs studied were satisfactory when compared with those obtained by ICP-OES. In the AM 1 tablet was obtained the content of 35.37% and 32.62% for TG by ICP-OES, at 6 AM a percentage of 17.77% and 16.82% and for AM 7 results obtained were 8.93% for both techniques, showing that the thermogravimetry can be used to determine the percentage of calcium in tablets. The technique offers speed, economy in the use of samples and procedures eliminating the use of acid reagents in the process of the sample and efficiency results.

Construção de modelos multivariados para determinação de lipídios totais e unidade em leite em pó comercial utilizando espectroscopia no infravermelho próximo

In this work calibration models were constructed to determine the content of total lipids and moisture in powdered milk samples. For this, used the near-infrared spectroscopy by diffuse reflectance, combined with multivariate calibration. Initially, the spectral data were submitted to correction of multiplicative light scattering (MSC) and Savitzsky-Golay smoothing. Then, the samples were divided into subgroups by application of hierarchical clustering analysis of the classes (HCA) and Ward Linkage criterion. Thus, it became possible to build regression models by partial least squares (PLS) that allowed the calibration and prediction of the content total lipid and moisture, based on the values obtained by the reference methods of Soxhlet and 105 ° C, respectively . Therefore, conclude that the NIR had a good performance for the quantification of samples of powdered milk, mainly by minimizing the analysis time, not destruction of the samples and not waste. Prediction models for determination of total lipids correlated (R) of 0.9955, RMSEP of 0.8952, therefore the average error between the Soxhlet and NIR was ± 0.70%, while the model prediction to content moisture correlated (R) of 0.9184, RMSEP, 0.3778 and error of ± 0.76%

Estudo do equilíbrio e cinética de adsorção de um corante aniônico em quitosana

The phenomenon of adsorption is of fundamental importance for the treatment of textile effluents and removal of dyes. Chitosan is characterized as an excellent adsorbent material, not only for its adsorption capacity but also the low cost production. Equilibrium and kinetic studies were developed in this study to describe the mechanism of adsorption of the anionic azo dye Orange G in chitosan, with the isotherms obtained from the variation of the concentration of dye in the continuous phase. The kinetics of the process was analyzed based on models involving the adsorption of molecules of the dye in nonpolar and polar sites. Adsorption experiments were carried out in water and in saline media with different NaCl concentrations, both for the determination of the equilibrium time as isotherms for making kinetic curves in which the amount of dye adsorbed measured indirectly varied with time. The experiments revealed the opening of the biopolymer structure with increasing concentration of Orange G, accompanied by high pH values and change on the type of interaction between the dye and the adsorbent surface, suggesting behavior advocated by the Langmuir equation in a certain range of concentration of the adsorbate and following the Henry's Law at higher concentrations, from the increased number of sites available for adsorption. The studies conducted showed that the saline medium reduces the chitosan s adsorption capacity according to a certain concentration, the occurrence of the cooperative adsorption process steps kinetic mechanism suggested as a new alternative for the interpretation of the phenomenon

Determinação do teor de diclofenaco sódico em comprimidos por espectroscopia no infravermelho próximo NIR com calibração multivariada PLS

This work is combined with the potential of the technique of near infrared spectroscopy - NIR and chemometrics order to determine the content of diclofenac tablets, without destruction of the sample, to which was used as the reference method, ultraviolet spectroscopy, which is one of the official methods. In the construction of multivariate calibration models has been studied several types of pre-processing of NIR spectral data, such as scatter correction, first derivative. The regression method used in the construction of calibration models is the PLS (partial least squares) using NIR spectroscopic data of a set of 90 tablets were divided into two sets (calibration and prediction). 54 were used in the calibration samples and the prediction was used 36, since the calibration method used was crossvalidation method (full cross-validation) that eliminates the need for a validation set. The evaluation of the models was done by observing the values of correlation coefficient R 2 and RMSEC mean square error (calibration error) and RMSEP (forecast error). As the forecast values estimated for the remaining 36 samples, which the results were consistent with the values obtained by UV spectroscopy

Determinação de Ba, Cd, Cr, Cu, Ni, Pb, Sn e Zn em Tainha (Mugil brasiliensis) nos estuários potiguares

Heavy metals can cause problems of human poisoning by ingestion of contaminated food, and the environment, a negative impact on the aquatic fauna and flora. And for the presence of these metals have been used for aquatic animals biomonitoramento environment. This research was done in order to assess the environmental impact of industrial and domestic sewage dumped in estuaries potiguares, from measures of heavy metals in mullet. The methods used for these determinations are those in the literature for analysis of food and water. Collections were 20 samples of mullet in several municipality of the state of Rio Grande do Norte, from the estuaries potiguares. Were analyzed the content of humidity, ash and heavy metals. The data were subjected to two methods of exploratory analysis: analysis of the main components (PCA), which provided a multivariate interpretation, showing that the samples are grouped according to similarities in the levels of metals and analysis of hierarchical groupings (HCA), producing similar results. These tests have proved useful for the treatment of the data producing information that would hardly viewed directly in the matrix of data. The analysis of the results shows the high levels of metallic species in samples Mugil brasiliensis collected in Estuaries /Potengi, Piranhas/Açu, Guaraíra / Papeba / Arês and Curimataú

Análises bromatológicas e fitoquímicas de frutos de Licania tomentosa (Benth) FRITSCH

This study conducted chemical analyzes of the fruits of Licania tomentosa Benth belonging to the Chrysobalanaceae family, order and superorder Rosiflorae Rosales. Samples were collected in February 2011 in the city of Natal - RN. The fruits were separated into peel, pulp and seed, and the samples were analyzed on moisture and ash by thermogravimetric methods, reducing and total sugars, lipids by Soxhlet extraction, minerals by ICP / OES and other analyzes by physical measurements of the fruit. The fruits for the analysis of determination of flavonoids and phenolic compounds were dried at 40 ° C and ground. For the analyzes to determine the content of phenolics and flavonols was used spectroscopy in the visible region, and also performed the characterization of ethanol extracts by high performance liquid chromatography and test for antioxidant activity hydroethanolic extracts. The results obtained are about 83.9% of the fruits have a length between 4.0 to 6.0 cm with respect to the diameter of the fruit about 97.4% of the fruits have a diameter between 2.0 - 4, 0 cm, mean weight of 36.14 g (7.86), the bark showed 60.5 (1.5)% relative humidity, the flesh 72.3 (0.9) and 44.4 seeds (0.4 )%, the bark showed 0.22 (0.00)% ash, the pulp 1.41 (0.01)% and the seed 1.18 (0.01)%, the bark showed 3.73 (0, 09) mg lipids / 100 g sample of the pulp 0.40 (0.04) and the seed 0.05 (0.00). With respect to reducing sugars and total gave the results, 16.23 (0.23) g/100g and 20.70 (0.24) g/100g. The fruit is presented with a good source of nutrients especially carbohydrates and lipids. The analysis for determining the antioxidant activity tests were performed reducing power and antioxidant capacity, the antioxidant capacity of hydroethanolic extracts of peel and pulp showed similar results, with higher concentrations however hydroethanolic bark extract. Regarding the content of phenolics and flavonoids hidroetanílico bark extract showed higher concentration values. The characterization of the extracts by high performance liquid chromatography identified the following compounds by retention time indicated by the race of the standards: galic acid, kaempferol and kaempferol derivatives. Considering the results of the fruit Licania tomentosa Benth may be an alternative food by analysis of their nutritional content and has substances with antioxidant action

Espectroscopia no infravermelho próximo e métodos de calibração multivariada aplicados à determinação simultânea de parâmetros bioquímicos em plasma sanguíneo

In this work, the quantitative analysis of glucose, triglycerides and cholesterol (total and HDL) in both rat and human blood plasma was performed without any kind of pretreatment of samples, by using near infrared spectroscopy (NIR) combined with multivariate methods. For this purpose, different techniques and algorithms used to pre-process data, to select variables and to build multivariate regression models were compared between each other, such as partial least squares regression (PLS), non linear regression by artificial neural networks, interval partial least squares regression (iPLS), genetic algorithm (GA), successive projections algorithm (SPA), amongst others. Related to the determinations of rat blood plasma samples, the variables selection algorithms showed satisfactory results both for the correlation coefficients (R²) and for the values of root mean square error of prediction (RMSEP) for the three analytes, especially for triglycerides and cholesterol-HDL. The RMSEP values for glucose, triglycerides and cholesterol-HDL obtained through the best PLS model were 6.08, 16.07 e 2.03 mg dL-1, respectively. In the other case, for the determinations in human blood plasma, the predictions obtained by the PLS models provided unsatisfactory results with non linear tendency and presence of bias. Then, the ANN regression was applied as an alternative to PLS, considering its ability of modeling data from non linear systems. The root mean square error of monitoring (RMSEM) for glucose, triglycerides and total cholesterol, for the best ANN models, were 13.20, 10.31 e 12.35 mg dL-1, respectively. Statistical tests (F and t) suggest that NIR spectroscopy combined with multivariate regression methods (PLS and ANN) are capable to quantify the analytes (glucose, triglycerides and cholesterol) even when they are present in highly complex biological fluids, such as blood plasma

Otimização de metodologias para determinação de hidrocarbonetos policíclicos aromáticos:aplicação em água do Rio Potengi

This work aims to detect polycyclic aromatic hydrocarbons (PAHs) through optimized analytical techniques, such as gas chromatography with flame-ionisation detector (CGFID), gas chromatography coupled to mass spectrometry (CGMS), Fluorescence Spectroscopy of Molecular and Purpot of oils and greases (POG). Apply to chemometrics, Factorial Planning 23, in the preparation of samples by liquid-liquid extraction. The sample preparation was used for liquid-liquid extraction and factors in this sample was used for the application of factorial planning 23, such as the use of ultrasound, solvents (dichloromethane, hexane and chloroform) and ratio of solvent / synthetic sample. These factors were assigned two types of levels: positive and negative. It was used to form the cube to better analyze the answers. The responses of the eight combinations were obtained in reading the spectrofluorimetric. The optimization of equipment were used, and they served in the HPA's identification of the samples collected in Rio Potengi. The optimization of the equipment was observed every 16's and PAH in the samples was found that the HPA's came from contamination of the Rio Potengi. The contamination comes through organic household waste, hospital waste, and among other contamination that comes from industries that are installed around the River The factorial design of high validity, it was observed a more effective sample preparation. The factorial design of liquid-liquid extraction showed a way to spend less solvent in less time using an ideal solvent, but also a way to extract more analyte from the matrix itself is water. In planning a smaller form factor extraction was the use of ultrasound, the ratio 1:3 corresponding to a solvent and sample 3 and the best solvent was dichloromethane who presented a viable extraction, not discarding the possibility of using also the hexane. The chloroform and may be toxic not had a good extraction

Espectrometria de emissão óptica com plasma indutivamente acoplado aliada à quimiometria na determinação de íons metálicos no molusco Mytella falcata para discriminação de estuários potiguares

This work examined the possibility of using mussel Mytella falcata as bioindicator sample to detect metal ions in several estuaries potiguares, since species substances that accumulate in their tissues due to its characteristics filter feeders have been used for environmental monitoring. The chemometrics by principal components analysis was used to reduce the size of the original data in order to establish a pattern of distribution of metal ion. Samples were collected at three different points in the estuaries Curimataú, Guaraíra-Papeba, Potengi, Galinhos-Guamaré and Piranhas-Assu having been marked with the location using GPS (Global Positioning System). The determination of humidity content and digestion of the samples were performed using methods described in the Compendium of analytical standards of the Institute Adofo Lutz (2005) and the determination of metal ions of the elements Al, Ba, Cd, Cr, Cu, Mn, Ni, Pb, Sn and Zn were performed by optical emission spectrometry with inductively coupled plasma as described by USEPA method 6010C. The results show that it is possible to use this molluscum Mytella falcata in the estuaries of Rio Grande do Norte for the determination of metal ions. The data were subjected to principal components analysis (PCA) which enabled us to verify the distribution pattern of the metal ions studied in several estuaries potiguares and group them according to the metal ions in common with and relate them to the activities in each region

Determinação de parâmetros (sólidos solúveis, pH e acidez titulável) em ameixas intactas usando espectroscopia no infravermelho próximo e seleção de comprimento de onda

The aim of this study was to evaluate the potential of near-infrared reflectance spectroscopy (NIRS) as a rapid and non-destructive method to determine the soluble solid content (SSC), pH and titratable acidity of intact plums. Samples of plum with a total solids content ranging from 5.7 to 15%, pH from 2.72 to 3.84 and titratable acidity from 0.88 a 3.6% were collected from supermarkets in Natal-Brazil, and NIR spectra were acquired in the 714 2500 nm range. A comparison of several multivariate calibration techniques with respect to several pre-processing data and variable selection algorithms, such as interval Partial Least Squares (iPLS), genetic algorithm (GA), successive projections algorithm (SPA) and ordered predictors selection (OPS), was performed. Validation models for SSC, pH and titratable acidity had a coefficient of correlation (R) of 0.95 0.90 and 0.80, as well as a root mean square error of prediction (RMSEP) of 0.45ºBrix, 0.07 and 0.40%, respectively. From these results, it can be concluded that NIR spectroscopy can be used as a non-destructive alternative for measuring the SSC, pH and titratable acidity in plums

Influência da densidade de carga e da massa molar da poliacrilamida na reologia de sistemas microemulsionados

The knowledge of the rheological behavior of microemulsionated systems (SME) is of fundamental importance due to the diversity of industrial applications of these systems. This dissertation presents the rheological behavior of the microemulsionated system formed by RNX 95/alcohol isopropyl/p-toulen sodium sulfonate/kerosene/distilled water with the addition of polyacrylamide polymer. It was chosen three polymers of the polyacrylamide type, which differ in molar weight and charge density. It was studied the addition of these polymers in relatively small concentration 0,1% in mass and maximum concentration of 2,0%. It was made analysis of flow to determine the appearing viscosities of the SME and rheological parameters applying Bingham, Ostwald de Waale and Herschell-Buckley models. The behavior into saline environment of this system was studied for a solution of KCl 2,0%, replacing the distilled water. It was determined the behavior of microemulsions in relation with the temperature through curves of flow in temperatures of 25 to 60ºC in variations of 5ºC. After the analysis of the results the microemulsion without the addition of polymer presented a slight increase in its viscosity, but it does not mischaracterize it as a Newtonian fluid. However the additive systems when analyzed with low concentration of polymer adjusted well to the applied models, with a very close behavior of microemulsion. The higher concentration of the polymer gave the systems a behavior of plastic fluid. The results of the temperature variation point to an increase of viscosity in the systems that can be related to structural changes in the micelles formed in the own microemulsion without the addition of polymer

Aplicação da termogravimetria na determinação do teor de ferro em comprimidos: um estudo comparativo com a espectrofotometria

This study used the Thermogravimetry (TG) and molecular absorption spectroscopy in UV-visible region to determine the iron content in herbal medicinal ferrous sulfate used in the treatment of iron deficiency anemia. The samples were characterized by IR, UV, TG / DTG, DTA, DSC and XRD. The thermoanalytical techniques evaluated the thermal stability and physicochemical events and showed that the excipients interfere in the decomposition of the active ingredients. The results of thermogravimetry showed that the decomposition temperature of the active principle Fe2(SO4)3 (T = 602 °C) is higher as compared to samples of tablets (566 586 °C). In the DTA and DSC curves were observed exothermic and endo events for samples of medicines and active analysis. The infrared spectra identified key functional groups exist in all samples of active ingredients, excipients and compressed studied, such as symmetric and asymmetric stretching of OH, CH, S=O. The analysis by X-ray diffraction showed that all samples had crystallinity and the final residue showed peaks indicating the presence of silicon dioxide, titanium dioxide and talc that are excipients contained in pharmaceutical formulations in addition to iron oxide. The results obtained by TG to determine the iron content of the studied drugs showed a variance when compared with those obtained by theoretical and UV-visible, probably due to formation of a mixture of Fe2O3 and Fe2(SO4)3. In one tablet was obtained FE content of 15.7 % and 20.6 % for TG by UV-visible, the sample EF 2 was obtained as a percentage of 15.4 % and 21.0 % for TG by UV-visible . In the third SF samples were obtained a content of 16.1 % and 25.5 % in TG by UV-visible, and SF 4 in the percentage of TG was 16.7 % and 14.3 % UV-visible