8 resultados para quantificação

em Repositorio Institucional da UFLA (RIUFLA)


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In the present study aimed to characterize and quantify four contaminants (ethyl carbamate, 2,3-butanedione, furfural and 5-hydroxymethylfurfural) present in alembic cachaça and industrial. Were collected forty-four samples of cachaça in the southern regions, the Midwest, southeast of Minas Gerais and São Paulo state, and subsequently subjected to physical, chemical and chromatographic analyzes. The physicochemical analyzes were performed according to the methodology described by the Ministry of Agriculture, Livestock and Supply (MAPA). The ethyl carbamate, 2,3-butanedione, furfuaral and 5 hydroxymethylfurfural were characterized and quantified by high-performance liquid chromatography (HPLC). The results of the ethyl carbamate analysis, it was found that both samples showed column cachaças outside the standards required by law, with the values 245.31 235.53 L-1 ug and none of the liquor samples alembic showed concentration greater than 210.0 ug L-1 , and the method is very sensitive to low limits of detection and quantification. In determining 2,3-butanedione, it was revealed that the column cachaças showed higher levels of contaminants when compared to cachaça alembic. In the quantification of furfural and 5-hydroxymethylfurfural was developed and validated analytical methods employed to high-performance liquid chromatography (HPLC) with DAD detector. Samples column cachaças showed higher values than the limit established by Brazilian legislation and ranged from 7.00 to 5.63 mg / 100 ml of anhydrous alcohol over the alembic cachaça.

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The objective of the present study was the evaluation of the presence of organic and inorganic contaminants in samples of aged cachaça from the South of the state of Minas Gerais. Furfural, methanol and copper were determined by colorimetric reactions, while the analyses of ethyl carbamate and acrolein were performed by GC/MS and HPLC, respectively. High levels of furfural and copper were obtained. All samples showed concentrations below the established by legislation for the ethyl carbamate, and for acrolein, only one sample showed higher levels. Methanol was not detected in the samples.

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The HPLC technique with UV-Vis detection was employed in the analysis of cocaine content in apprehended samples of cocaine and crack. A peak signal for cocaine was obtained in 3.5 minutes run by using acetonitrile/water (95:5v/v) as a mobile phase. Optimized spectrophotometric signal was obtained at a wavelength of 224 nm. The analytical curve from 1.0 to 40.0 ppm of cocaine was obtained, showing a linear correlation coefficient of 0.9989, with detection and quantification limits of 0.75 ppm and 3.78 ppm, respectively. This methodology was employed at the dosage of confiscated samples of cocaine and crack in the Scientific Police Laboratory of Ribeirão Preto-SP city.

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The barks generated from the wood processing industries are wastes generated in significant quantities, becoming interesting to have basic studies of their anatomical and chemical properties in order to make better use of this material. This study aimed to carry out anatomical studies, chemical and tannins from the barks of commercial clones of Eucalyptus. For this, permanent histological slides for anatomical characterization and percentage of cellular elements were prepared; and cellular elements were dissociated for biometry of the elements. The analyses were related to chemical extractives, ash, lignin, suberin, sugars, phenols, tannins, flavonoids and antioxidant activity of the extracts. The tannins were extracted in pure water and with water mixed with sodium sulfite, and were subsequently evaluated the properties by FT-IR. It was verified by the anatomical characterization and chemical quantification, the similarity between the clones. Regarding the biometrics of cellular elements, statistically significant differences were not observed for the following parameters: length and diameter of sieve tube, axial parenchyma diameter, and rays hight. The yield of condensed tannins and Stiasny index for studied clones are low, showing the infeasibility of using bark for the extraction of tannins to produce adhesives, however tannins and other bioactive phenolic compounds can be used in the pharmaceutical and cosmetics sectors due to its antioxidant potential. The spectrum of tannins is the same as the one found the literature. Due to the high yield of verified sugar, (around 46,68%) sugars are potencial products, with a high yield of glucose , it is interesting for application in biorefinery.

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Different solvents were evaluated for the extraction of jabuticaba anthocyanin pigments, identifying, quantifying and verifying the stability of the anthocyanins, as well as the conduction of three antioxidant activity assays and determination of the vitamin C levels. The maceration with ethanol acidified with HCl 1.5 mol L-1 (85:15) provides better pigment extraction and stability. The skin is anthocyanin rich, presenting 1.59 and 2.06 g 100 g-1 of dry matter in the Paulista and Sabará varieties, respectively. Cyanidin 3-glucoside is the majority pigment of the skins, followed by delphinidin 3-glucoside. The highest level of vitamin C was found in the skins and seeds of both varieties. It was verified that the skins, presented more antioxidant activity, in free radical capture, as well as in retarding the lipid oxidation process.

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The development of an electroanalytical method for simultaneous determination of copper and lead ions in sugar cane spirit (cachaça) using carbon paste electrode modified with ascorbic acid and carbon nanotubes (CPE-AaCNT) is described. Squarewave voltammetry (SWV) with anodic stripping was employed, and this technique was optimized with respect to the following parameters: frequency (50 Hz), amplitude (100 mV) and scan increment (9 mV). The analytical curves were linear in the range from 0.0900 to 7.00 mg L - 1 for lead and copper. The limits of detection were 48.5 and 23.9 µg L - 1 for lead and copper, respectively. The developed method was applied to the simultaneous determination of copper and lead in five commercial samples of sugar cane spirit. The results were in good agreement with those obtained by F AAS/GF AAS (flame atomic absorption spectrometry/graphite furnace atomic absorption spectrometry) and showed that CPE-AaCNT can be successfully employed in the simultaneous determination of these metals in real sugar cane spirit samples.

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The objective of this study was to characterize phenolic compounds and evaluate the effect, under laboratory conditions, of the cassava leaf powder methanol extract on the development of fall armyworm Spodoptera frugiperda and of leaf-cutting ant Atta sexdens rubropilosa. The extract was incorporated into an artificial diet, to which the armyworm was exposed, at concentrations of 250, 500, 1000 and 1500 mg kg-1,in order to evaluate biological characteristics. Soon after the insects emergence, another experiment was conducted to verify the possible sub lethal activity of the extract; therefore, S. frugiperda couples were isolated in cages and eggs were collected and counted. The Manihot esculenta Crantz extract caused a reduction in the percentage of armyworm survival, as well as in the eggs number. Then, the same extract was solubilized in 10% ethanol and applied to ants; mortality was observed, compared to the control. It is possible to conclude that the M. esculenta Crantz leaf powder methanolic extract, containing gallic acid and catechin, is a promising alternative to control S. frugiperda and Atta sexdens rubropilosa.

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Sugar is widely consumed worldwide and Brazil is the largest producer, consumer, and exporter of this product. To guarantee proper development and productivity of sugar cane crops, it is necessary to apply large quantities of agrochemicals, especially herbicides and pesticides. The herbicide tebuthiuron (TBH) prevents pre- and post-emergence of infesting weed in sugarcane cultures. Considering that it is important to ensure food safety for the population, this paper proposes a reliable method to analyse TBH in sugar matrixes (brown and crystal) using square wave voltammetry (SWV) and differential pulse voltammetry (DPV) at bare glassy carbon electrode and investigate the electrochemical behavior of this herbicide by cyclic voltammetry (CV). Our results suggest that TBH or the product of its reaction with a supporting electrolyte is oxidized through irreversible transfer of one electron between the analyte and the working electrode, at a potential close to +1.16 V vs. Ag |AgClsat in 0.10 mol L-1 KOH as supporting electrolyte solution. Both DPV and SWV are satisfactory for the quantitative analysis of the analyte. DPV is more sensitive and selective, with detection limits of 0.902, 0.815 and 0.578 mg kg-1, and quantification limits of 0.009, 0.010 and 0.008 mg kg-1 in the absence of the matrix and in the presence of crystal and brown sugar matrix, respectively. Repeatability lay between 0.53 and 13.8%, precision ranged between 4.14 and 15.0%, and recovery remained between 84.2 and 113% in the case of DPV conducted in the absence of matrix and in the presence of the crystal sugar matrix, respectively.