Screening Brazilian commercial gasoline quality by hydrogen nuclear magnetic resonance spectroscopic fingerprintings and pattern-recognition multivariate chemometric analysis

The identification of gasoline adulteration by organic solvents is not an easy task, because compounds that constitute the solvents are already in gasoline composition. In this work, the combination of Hydrogen Nuclear Magnetic Resonance ((1)H NMR) spectroscopic fingerprintings with pattern-recognition multivariate Soft Independent Modeling of Class Analogy (SIMCA) chemometric analysis provides an original and alternative approach to screening Brazilian commercial gasoline quality in a Monitoring Program for Quality Control of Automotive Fuels. SIMCA was performed on spectroscopic fingerprints to classify the quality of representative commercial gasoline samples selected by Hierarchical Cluster Analysis (HCA) and collected over a 6-month period from different gas stations in the São Paulo state, Brazil. Following optimized the (1)H NMR-SIMCA algorithm, it was possible to correctly classify 92.0% of commercial gasoline samples, which is considered acceptable. The chemometric method is recommended for routine applications in Quality-Control Monitoring Programs, since its measurements are fast and can be easily automated. Also, police laboratories could employ this method for rapid screening analysis to discourage adulteration practices. (C) 2010 Elsevier B.V. All rights reserved.

Método de análise isotópica (δ13C) e limite de legalidade em néctar de laranja

Os objetivos deste trabalho foram desenvolver o método de análise isotópica para quantificar o carbono do ciclo fotossintético C3 em néctares de laranja comerciais e mensurar o limite de legalidade, baseado na legislação brasileira, para identificar as bebidas que não estão em conformidade com o Ministério da Agricultura, Pecuária e Abastecimento (MAPA). As bebidas foram produzidas em laboratório, conforme a legislação brasileira. Também foram produzidos néctares adulterados com quantidade de suco de laranja abaixo do limite mínimo permitido pelo MAPA. Na análise isotópica, foi mensurado o enriquecimento isotópico relativo dos néctares de laranja e também de suas frações, sólidos insolúveis (polpa) e açúcar purificado. Com esses resultados, foi estimada a quantidade de fonte C3 por meio da equação da diluição isotópica. Para determinar a existência de adulteração, foi necessária a criação do limite de legalidade de acordo com a legislação brasileira. Oito marcas comerciais de néctar de laranja foram analisadas. Todas foram classificadas como legais. O limite de legalidade foi uma importante inovação metodológica, que possibilitou identificar as bebidas que estavam em conformidade com a legislação brasileira. A metodologia desenvolvida provou ser eficiente para quantificar o carbono de origem C3 em néctares de laranja comerciais.

Análise isotópica (δ13C) e legalidade em suco e polpa de caju

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

Carbon isotope analysis in apple nectar beverages

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

Último Desejo e Testamento de Wilhelm Reich

O objetivo desta tradução é contribuir para a divulgação do pensamento do médico psiquiatra e inicialmente, psicanalista, Wilhelm Reich. Nascido em 24 de março de 1897, em parte da Galícia pertencente ao Império austro-húngaro, Reich morreu na prisão em 03 de novembro de 1957 nos Estados Unidos da América. Contudo, poucos meses antes do ataque cardíaco que o levou à morte, Reich legou sua obra às crianças do futuro em testamento assinado em 08 de março de 1957, onde registrou seus últimos desejos sob o testemunho de Willian Moise, Michael Silvert e Willian Steig, temendo possíveis distorções, difamações, adulterações e destruição de seus escritos após a sua morte.

Determinação do percentual de malte e adjuntos em cervejas comerciais brasileiras através de análise isotópica

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

Rapid spot test analysis for the detection of urotropine in pharmaceutical preparations

The widespread falsification and/or adulteration of commercially available pharmaceutical preparations call for reliable methods of drug identification, preferably through selective and rapid sorting color tests that could be undertaken with minimum equipment remote from laboratory facilities. The present work deals with a convenient adaptation and refinement of a spot test devised by Feigl (1966) for urotropine, based on the hydrolytic cleavage of that substance in the presence of sulfuric acid, splitting out formaldehyde which is identified by its color reaction with chromotropic acid. A simple emergency kit was developed for the quick, efficient, inexpensive and easy performance of urotropine tests by semiskilled personnel even in the drugstore laboratory (or office) as well as in a mobile screening operation. It is shown that when the reagents are added according to the recommended sequence a self-heating system is generated, increasing substantially the reactions' rates and the test sensitivity as well. The identification limit found was 25 mug of urotropine, for both solid and liquid samples. The possible interference of 84 substances/materials was investigated. Interference was noted only for methylene blue, acriflavine, Ponceau Red, Bordeaux Red (these dyes are often included in urotropine dosage forms), pyramidone, dipyrone, quinine and tetracycline. A simple procedure for removing most of the interferences is described. Data for 8 commercial dosage forms and results obtained from their analysis are presented.

Correlation between acidic ninhydrin and HPLC methods to evaluate fraudulent addition of whey in milk

The acidic ninhydrin spectrophotometric method (ANSM) for quantitative determination of free and bound sialic acid of milk glycoprotein has been proved to be fast and efficient for routine detection of fraudulent addition of rennet whey to fluid milk. In this research the ANSM was compared with the high performance liquid chromatography (HPLC) method, internationally recommended for caseinomacropeptide (CMP) determination, which besides its high accuracy is more sophisticated and requires trained personnel. For several sample conditions (raw milk and milk with variable added amounts of rennet cheese whey), the methods showed an excellent linear correlation, with r = 0.981 when milk was deproteinized with a 120 g.L-1 final concentration of trichloroacetic acid (TCA) concentration. The best correlations could be seen with final concentrations of 100 g.L-1 and 80 g.L-1 TCA; respectively, r = 0.992 and 0.993.

Screening Brazilian automotive gasoline quality through quantification of saturated hydrocarbons and anhydrous ethanol by gas chromatography and exploratory data analysis

In this paper a set of Brazilian commercial gasoline representative samples from São Paulo State, selected by HCA, plus six samples obtained directly from refineries were analysed by a high-sensitive gas chromatographic (GC) method ASTM D6733. The levels of saturated hydrocarbons and anhydrous ethanol obtained by GC were correlated with the quality obtained from Brazilian Government Petroleum, Natural Gas and Biofuels Agency (ANP) specifications through exploratory analysis (HCA and PCA). This correlation showed that the GC method, together with HCA and PCA, could be employed as a screening technique to determine compliance with the prescribed legal standards of Brazilian gasoline.

Screening Brazilian C gasoline quality: Application of the SIMCA chemometric method to gas chromatographic data

A total of 2400 samples of commercial Brazilian C gasoline were collected over a 6-month period from different gas stations in the São Paulo state, Brazil, and analysed with respect to 12 physicochemical parameters according to regulation 309 of the Brazilian Government Petroleum, Natural Gas and Biofuels Agency (ANP). The percentages (v/v) of hydrocarbons (olefins, aromatics and saturated) were also determined. Hierarchical cluster analysis (HCA) was employed to select 150 representative samples that exhibited least similarity on the basis of their physicochemical parameters and hydrocarbon compositions. The chromatographic profiles of the selected samples were measured by gas chromatography with flame ionisation detection and analysed using soft independent modelling of class analogy (SIMCA) method in order to create a classification scheme to identify conform gasolines according to ANP 309 regulation. Following the optimisation of the SIMCA algorithm, it was possible to classify correctly 96% of the commercial gasoline samples present in the training set of 100. In order to check the quality of the model, an external group of 50 gasoline samples (the prediction set) were analysed and the developed SIMCA model classified 94% of these correctly. The developed chemometric method is recommended for screening commercial gasoline quality and detection of potential adulteration. (c) 2007 Elsevier B.V. All rights reserved.

β-casein gene polymorphism permits identification of bovine milk mixed with bubaline milk in mozzarella cheese

Mozzarella cheese is traditionally prepared from bubaline (Bubalus bubalis) milk, but product adulteration occurs mainly by addition of or full substitution by bovine milk. The aim of this study was to show the usefulnes of molecular markers to identify the admixture of bovine milk to bubaline milk during the manufacturing process of mozzarella cheese. Samples of mozzarella cheese were produced by adding seven different concentrations of bovine milk: 0%, 1%, 2%, 5%, 8%, 12% and 100%. DNA extracted from somatic cells found in cheese were submitted to PCR-RFLP analysis of casein genes: α-s1-CN - CSN1S1 that encompasses 954 bp from exon VII to intron IX (AluI and HinfI), β-CN - CSN2 including 495 bp of exon VII (Hae III and HinfI), and κ-CN - CSN3, encompassing 373 bp of exon IV (AluI and HindIII). Our results indicate that Hae III-RFLP of CSN2exon VII can be used as a molecular marker to detect the presence of bovine milk in mozzarella cheese. Copyright © 2008, Sociedade Brasileira de Genética.

Análise isotópica (δ13c) e legalidade em néctares de uva

The aim of this work was to develop an isotopic analysis method to quantify the carbon of C3 photosynthesis cycle in grape nectar and to identify the commercial beverages in disagreement to the Brazilian Ministry of Agriculture, Livestock and Food Supply (MAPA) regulation. The nectars were produced in a laboratory, according to the Brazilian Law. Adulterated beverages with quantity of grape juice lower than the legal limit were also produced. Isotopic analysis measured the relative isotopic enrichment of grape nectar and its purified sugar fraction. Based on these results, it was possible to estimated the quantity of source C3 by means of isotopic dilution equation. To determine the existence of adulteration in commercial nectars, it was necessary to create a legal limit according to the Brazilian Law. One of the twelve commercial brands of nectar analyzed was classified as adulterated. The developed methodology proved to be efficient to quantify the carbon of C3 origin and identify the adulterated commercial grape nectar.

Caracterização de leite utilizando técnicas de ultra-som e redes neurais

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Análise isotópica da variabilidade natural do carbono-13 e avaliação energética em néctares de pêssego – Prunus persica (L.) Batsch

Pós-graduação em Agronomia (Energia na Agricultura) - FCA

Estudo da microestrutura e da resistência à corrosão integranular em chapas soldadas de aços inoxidáveis austeníticos série 304L após goivagem ao arco elétrico

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)