212 resultados para procedimentos analíticos
Resumo:
A review of polypeptides and proteins that influence, direct or indirectly, beer foam quality, as well as the most relevant analytical methods used in their study, are presented. Protein Z, LTP1 and hordein/glutelin fragments originated from malt have a direct influence on beer foam quality. Other proteins, like malt hordeins and albumins and wheat puroindolines, are, to some degree, also important for beer foam quality. Protein hydrophobicity is pointed out as a key parameter to enhance foam quality. Electrophoretic, chromatographic and immunological analytical methods are currently used to study polypeptides and proteins present in barley, malt, wort, beer, and foam. Best results are obtained when combinations of these methods are applied.
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We review here the chemistry of reactive oxygen and nitrogen species, their biological sources and targets; particularly, biomolecules implicated in the redox balance of the human blood, and appraise the analytical methods available for their detection and quantification. Those biomolecules are represented by the enzymatic antioxidant defense machinery, whereas coadjutant reducing protection is provided by several low molecular weight molecules. Biomolecules can be injured by RONS yielding a large repertoire of oxidized products, some of which can be taken as biomarkers of oxidative damage. Their reliable determination is of utmost interest for their potentiality in diagnosis, prevention and treatment of maladies.
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This work presents the VALIDATION SPREADSHEET, a public domain tool that can be used to evaluate the figures of merit for univariate analytical methods. A real example of BTEX determination in environmental samples is included to illustrate its use. The spreadsheet has been developed for Excel® and Open Office®, and is available on the internet at http//lqta.iqm.unicamp.br.
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Extraction and clean-up are essential points in polycyclic aromatic hydrocarbon (PAHs) analysis in a solid matrix. This work compares extraction techniques and clean-up procedures for PAH analysis. PAH levels, their toxicological significance and source were also evaluated in the waters of the Cocó and Ceará rivers. The efficiency of PAH recovery was higher for the soxhlet and ultrasonic techniques. PAH recovery varied from 69.3 to 99.3%. Total PAH concentration (ΣHPA) varied from 720.73 to 2234.76 µg kg-1 (Cocó river) and 96.4 to 1859.21 µg kg-1 (Ceará river). The main PAH sources are pyrolytic processes and the levels were classified as medium so that adverse effects are possible.
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Plastic packaging materials intended for use in food packaging is an area of great interest from the scientific and economic point of view due to the irreversible internationalization and globalization process of food products. Nevertheless, a debate related to food safety aspects has emerged within the scientific community. Therefore, the development of analytical methods that allow identifying and quantifying chemical substances of toxicological potential in the packaging is considered essential. This article focuses on the main analytical methods, including validation parameters, as well as extraction and quantification techniques for determination of volatile organic compounds from food packaging materials.
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In this work is proposed, a simple experiment for the simultaneous determination of losartan (L) and hydrochlorothiazide (H) in synthetic and real samples by derivative spectrophotometry technique. For the students it is relevant to know this technique for simultaneous determinations of drugs, allowing that the students recognize that this technique is simple, rapid and applicable to quality control. This experimental work, it is proposed in order to being applied to undergraduates into laboratories of analytical chemistry. Furthermore, it is given the integration of the theoretical knowledge with the experimental work; this correlation is of interest for the students.
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The establishment of quality standards for biodiesel was a key step to win the confidence of the market and the automotive industry, thus ensuring the success of the new fuel. In this review are presented standard methods and other analytical methods suggested for analysis of biodiesel. The methods of analysis were divided into groups according to information that may be provided on the contaminants from the raw material of the production process, the molecular structures of biodiesel and its degradation during storage.
Resumo:
Three analytical methods for the determination of BTEX in water were optimized and validated. With the best method the analytes were extracted of 10 mL of sample with 2.50 g of NaCl in headspace vial of 20 mL by HS and SPME to 40 ºC for 30 min for adsorption and to 250 ºC for 4 min for desorption and were analyzed by GC-MS. The recovery was between 97.9% and 104.3%, and the limit of detection was 2.4 ng L-1 for o-xylene. This method was using to analyze BTEX in water supply and surface water in Ouro Preto city. No sample had concentrations of BTEX above the legislation.
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The development of analytical methods for determination of eight pesticides of different chemical classes (trichlorfon, propanil, fipronil, propiconazole, trifloxystrobin, permethrin, difenoconazole and azoxystrobin) in sediments with gas chromatography-micro-electron capture detector (GC/µECD) and comprehensive two-dimensional gas chromatography with micro-electron capture detector (GCxGC/µECD) is described. These methods were applied to real sediment samples, and the best results were obtained using a 5% diphenyl-methylpolysiloxane column for 1D-GC. For GCxGC the same column was employed in the first dimension and a 50%-phenyl-methylpolysiloxane stationary phase was placed in the second dimension. Due to the superior peak capacity and selectivity of GCxGC, interfering matrix peaks were separated from analytes, showing a better performance of GCxGC.
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The variability in aflatoxin B1 concentration among peanut subsamples of 4 sample preparation procedures was evaluated. For each procedure, 18 samples were prepared involving dry comminuting/homogenization or dry roughly comminuting followed by the preparation of a aqueous slurry. Ten analytical samples were withdrawn from each sample/procedure and analyzed by thin layer chromatography. The coefficient of variation (CV%) among each set of 10 analytical samples was assumed to be associated with the sample preparation procedure. The procedure that made use of a subsample mill and preparation of a subsample slurry, showed lower variability (CV%) among the analytical subsamples.
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The use of dyes in the commercialization of fuel is usually associated with protection of the source and destination. It is used as "markers" to identify and guarantee the identity of the specific product of a particular manufacturer to discourage theft, tampering and disclosure of the quality of solvent or fuel. This work presents a critical analysis on the state of the art about the available analytical methods for identification and quantification of dyes used as markers of solvents and fuels, as well as evaluation of the physical-chemical staining and laws surrounding their use and commercialization.
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In this review recent methods developed and applied to solve criminal occurences related to documentoscopy, ballistic and drugs of abuse are discussed. In documentoscopy, aging of ink writings, the sequence of line crossings and counterfeiting of documents are aspects to be solved with reproducible, fast and non-destructive methods. In ballistic, the industries are currently producing ''lead-free'' or ''nontoxic'' handgun ammunitions, so new methods of gunshot residues characterization are being presented. For drugs analysis, easy ambient sonic-spray ionization mass spectrometry (EASI-MS) is shown to provide a relatively simple and selective screening tool to distinguish m-CPP and amphetamines (MDMA) tablets, cocaine and LSD.
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In the recent years, analytical toxicologists have been facing difficulties in detecting designer drugs due to the chemical modifications on the existing structures and the speed in which they are released into the market, requiring the development and improvement of specific and appropriate analytical methods. This work is a review of the literature which summarizes the characteristics of the drugs and the analytical validated methods using conventional and unconventional matrices currently used for correct identification and quantification of the following classes of emerging drugs of abuse: derivatives of opiates, amphetamines, tryptamines, piperazines and cannabinoids.
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The analysis of fatty acid (FA) esters by gas chromatography and flame ionization detector (FID) normally uses the normalization method. However, if one FA is wrongly estimated, the results could be greatly affected. In this study, methodologies using internal standards and correction factors for the FID response are described. The results show that by using theoretical correction factors associated to the internal standardization, the quantitative analyses of the FAs are expressed in mass, increasing the accuracy and facilitating the interpretation and comparison of the results for foods and biodiesels.
Resumo:
Interest in analytical methods for quality control of herbal drugs has grown sharply due to the scarcity of monographs in official manuals. Thus, the aim of the present study was to evaluate analytical procedures for quantitative determination of flavonoids from leaves of Bauhinia forficata Link (pata-de-vaca). Two procedures for quantification of total flavonoids (with and without acid hydrolysis) by spectrophotometry were tested. The proposed methods proved to be specific, sensitive, precise, accurate and robust, being suitable for routine laboratory use.