Profiling allergic asthma volatile metabolic patterns using a headspace-solid phase microextraction/gas chromatography based methodology

Allergicasthmarepresentsanimportantpublichealthissuewithsignificantgrowthovertheyears,especially in the paediatric population. Exhaled breath is a non-invasive, easily performed and rapid method forobtainingsamplesfromthelowerrespiratorytract.Inthepresentmanuscript,themetabolicvolatile profiles of allergic asthma and control children were evaluated by headspace solid-phase microextraction combined with gas chromatography–quadrupole mass spectrometry (HS-SPME/GC–qMS). The lack ofstudiesinbreathofallergicasthmaticchildrenbyHS-SPMEledtothedevelopmentofanexperimental design to optimize SPME parameters. To fulfil this objective, three important HS-SPME experimental parameters that influence the extraction efficiency, namely fibre coating, temperature and time extractions were considered. The selected conditions that promoted higher extraction efficiency corresponding to the higher GC peak areas and number of compounds were: DVB/CAR/PDMS coating fibre, 22◦C and 60min as the extraction temperature and time, respectively. The suitability of two containers, 1L Tedlar® bags and BIOVOC®, for breath collection and intra-individual variability were also investigated. The developed methodology was then applied to the analysis of children exhaled breath with allergicasthma(35),fromwhich13hadalsoallergicrhinitis,andhealthycontrolchildren(15),allowing to identify 44 volatiles distributed over the chemical families of alkanes (linear and ramified) ketones, aromatic hydrocarbons, aldehydes, acids, among others. Multivariate studies were performed by Partial LeastSquares–DiscriminantAnalysis(PLS–DA)usingasetof28selectedmetabolitesanddiscrimination between allergic asthma and control children was attained with a classification rate of 88%. The allergic asthma paediatric population was characterized mainly by the compounds linked to oxidative stress, such as alkanes and aldehydes. Furthermore, more detailed information was achieved combining the volatile metabolic data, suggested by PLS–DA model, and clinical data.

A sensitive microextraction by packed sorbent-based methodology combined with ultra-high pressure liquid chromatography as a powerful technique for analysis of biologically active flavonols in wines

A new approach based on microextraction by packed sorbent (MEPS) and reversed-phase high-throughput ultra high pressure liquid chromatography (UHPLC) method that uses a gradient elution and diode array detection to quantitate three biologically active flavonols in wines, myricetin, quercetin, and kaempferol, is described. In addition to performing routine experiments to establish the validity of the assay to internationally accepted criteria (selectivity, linearity, sensitivity, precision, accuracy), experiments are included to assess the effect of the important experimental parameters such as the type of sorbent material (C2, C8, C18, SIL, and C8/SCX), number of extraction cycles (extract-discard), elution volume, sample volume, and ethanol content, on the MEPS performance. The optimal conditions of MEPS extraction were obtained using C8 sorbent and small sample volumes (250 μL) in five extraction cycle and in a short time period (about 5 min for the entire sample preparation step). Under optimized conditions, excellent linearity View the MathML source(Rvalues2>0.9963), limits of detection of 0.006 μg mL−1 (quercetin) to 0.013 μg mL−1 (myricetin) and precision within 0.5–3.1% were observed for the target flavonols. The average recoveries of myricetin, quercetin and kaempferol for real samples were 83.0–97.7% with relative standard deviation (RSD, %) lower than 1.6%. The results obtained showed that the most abundant flavonol in the analyzed samples was myricetin (5.8 ± 3.7 μg mL−1). Quercetin (0.97 ± 0.41 μg mL−1) and kaempferol (0.66 ± 0.24 μg mL−1) were found in a lower concentration. The optimized MEPSC8 method was compared with a reverse-phase solid-phase extraction (SPE) procedure using as sorbent a macroporous copolymer made from a balanced ratio of two monomers, the lipophilic divinylbenzene and the hydrophilic N-vinylpyrrolidone (Oasis HLB) were used as reference. MEPSC8 approach offers an attractive alternative for analysis of flavonols in wines, providing a number of advantages including highest extraction efficiency (from 85.9 ± 0.9% to 92.1 ± 0.5%) in the shortest extraction time with low solvent consumption, fast sample throughput, more environmentally friendly and easy to perform.

Análise topológica experimental por perfilometria cíclica indutiva de superficies de paredes estruturais

To enhance the maintenance practices, Oil and Gas Pipelines are inspected from the inside by automated systems called PIG (Pipeline Inspection Gauge). The inspection and mapping of defects, as dents and holes, in the internal wall of these pipelines are increasingly put into service toward an overall Structural Integrity Policy. The residual life of these structures must be determined such that minimize its probability of failure. For this reason, the investigation on the detection limits of some basic topological features constituted by peaks or valleys disposed along a smooth surface is of great value for determining the sensitivity of the measurements of defects from some combinations of circumferential, axial and radial extent. In this investigation, it was analyzed an inductive profilometric sensor to scan three races, radius r1, r2, r3, in a circular surface of low carbon steel, equipped with eight consecutive defects simulated by bulges and holes by orbit, equally spaced at p/4 rad. A test rig and a methodology for testing in laboratory were developed to evaluate the sensor response and identify their dead zones and jumps due to fluctuations as a function of topological features and scanning velocity, four speeds different. The results are presented, analyzed and suggestions are made toward a new conception of sensor topologies, more sensible to detect these type of damage morphologies

Comparação entre planejamento estatístico experimental e análise dimensional em operações de mistura e separação para sistema óleo-água

This work aims to determine a better methodology to help predicting some operational parameters to a new design of mixer-settler on treating wastewater produced by petroleum industry, called MDIF (Misturador-Decantador à Inversão de Fases/ Mixer-Settler based on Phase Inversion MSPI). The data from this research were obtained from the wastewater treatment unit, called MSPI-TU, installed on a wastewater treatment plant (WTP) of PETROBRAS/UO-RNCE. The importance in determining the better methodology to predict the results of separation and extraction efficiency of the equipment, contributes significantly to determine the optimum operating variables for the control of the unit. The study was based on a comparison among the experimental efficiency (E) obtained by operating MSPI-TU, the efficiency obtained by experimental design equation (Eplan) from the software Statistica Experimental Design® (version 7.0), and the other obtained from a modeling equation based on a dimensional analysis (Ecalc). The results shows that the experimental design equation gives a good prediction of the unit efficiencies with better data reliability, regarding to the condition before a run operation. The average deviation between the proposed by statistic planning model equation and experimental data was 0.13%. On the other hand, the efficiency calculated by the equation which represents the dimensional analysis, may result on important relative deviations (up 70%). Thus, the experimental design is confirmed as a reliable tool, with regard the experimental data processing of the MSPI-TU

Quantification of bovine cytokine gene expression using real-time RT-PCR methodology

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

Optimization of cyclodextrin glucanotransferase production from Bacillus clausii E16 in submerged fermentation using response surface methodology

Cyclodextrin glucanotransferase production from Bacillus clausii E16, a new bacteria isolated from Brazilian soil samples was optimized in shake-flask cultures. A 2 4 full-factorial central composite design was performed to optimize the culture conditions, using a response surface methodology the combined effect among the soluble starch concentration, the peptone concentration, the yeast extract concentration, and the initial pH value of the culture medium was investigated. The optimum concentrations of the components, determined by a 2(4) full-factorial central composite design, were 13.4 g/L soluble starch, 4.9 g/L peptone, 5.9 g/L yeast extract, and initial pH 10.1. Under these optimized conditions, the maximum cyclodextrin glucanotransferase activity was 5.9 U/mL after a 48-h fermentation. This yield was 68% higher than that obtained when the microorganism was cultivated in basal culture medium.

Optimization of xylanase production by Bacillus circulans D1 in submerged fermentation using response surface methodology

In this work, a 3(3) factorial design was performed with the aim of optimizing the culture conditions for xylanase production by an alkalophilic thermophilic strain of Bacillus circulans, using response surface methodology. The variables involved in this study were xylan concentration (X-1), pH (X-2) and cultivation time (X-3). The optimal response region was approached without using paths of steepest ascent. Statistical analysis of results showed that, in the range studied, only pH did not have a significant effect on xylanase production. A second-order model was proposed to represent the enzymic activity as a function of xylan concentration (X-1) and cultivation time (X-3). The optimum xylan concentration and cultivation time were 5 g/l and 48 h, respectively. Under these conditions, the model predicted a xylanase activity of 19.1 U/ml. (C) 2002 Elsevier B.V. Ltd. All rights reserved.

Joint Experimental and Theoretical Analysis of Order Disorder Effects in Cubic BaZrO3 Assembled Nanoparticles under Decaoctahedral Shape

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

A Contribution to the Estimation of Binary Halide and Pseudo-Halide Equilibrium Constants using a Linear Extrapolation Methodology

The molar single ion activity coefficient (y(F)) of fluoride ions was determined at 25 degrees C and ionic strengths between 0.100 and 3.00 mol L(-1) NaClO(4) using an ion-selective electrode. The activity coefficient dependency on ionic strength was determined to be Phi(F) = log y(F) = 0.2315I-0.041I(2). The function Phi(F)(I), combined with functions obtained in previous work for copper (Phi(Cu)) and hydrogen (Phi(H)), allowed us to make the estimation of the stoichiometric and thermodynamic protonation constants of some halides and pseudo-halides as well as the formation constants of some pseudo-halides and fluoride 1:1 bivalent cation complexes. The calculation procedure proposed in this paper is consistent with critically-selected experimental data. It was demonstrated that it is possible to use Phi(F)(I) for predicting the thermodynamic equilibrium parameters independently of Pearson's hardness of acids and bases.

Método experimental para determinação das capacitancias parasitas do motor de indução trifásico acionado por inversor MLP

A proposta deste trabalho é apresentar uma nova metodologia para determinação experimental das capacitancias parasitas do motor de indução trifásico de rotor em gaiola. As capacitancias parasitas fazem parte do circuito equivalente do motor para estudos de interferência eletromagnética causada no motor de indução em modo comum quando ele for acionado por inversor controlado por modulação por largura de pulsos (MLP). Os procedimentos propostos para o desenvolvimento deste novo método consistem em: a) determinação dos parâmetros do circuito equivalente do motor de indução trifásico, em regime permanente, através de ensaio em laboratório; b) estabelecer configurações de ligações entre o inversor MLP e o motor para medições das grandezas de interesse que são as seguintes: tensões de modo comum e de eixo, correntes de fuga e de eixo, através de circuito de medição desenvolvido para este fim; c) calcular os valores das capacitancias parasitas entre estator e carcaça do motor; estator e rotor; rotor e carcaça e de rolamento utilizando a expressão matemática da definição de capacitancia; d) utilizar o software Pspice para simular o sistema motor de indução trifásico, alimentado por inversor MLP, com os circuitos equivalentes em baixas e altas frequências; e) obter as formas de onda características do fenômeno de modo comum.

Metodologia experimental para avaliação de custos de produção e utilização de biodiesel: estudo de caso de quatro ésteres metílicos e óleo diesel comercial

Considerando que o Brasil detém uma vasta gama de matérias-primas para produção de biodiesel, e também que há a possibilidade de produção em pequena escala, prima-se por estudos de cunho econômico a partir de metodologias de fácil execução. O objetivo do trabalho foi demonstrar uma metodologia e sua aplicação para avaliação dos custos inseridos dentro do processo produtivo e de utilização do biodiesel. A metodologia foi aplicada a biodieseis originários de óleo de soja, girassol, frango e sebo bovino, dos quais se avaliaram economicamente os custos fixos e variáveis para conversão química dos óleos e gorduras em ésteres metílicos, em uma planta de produção experimental. Os custos de produção para cada uma das quatro citadas são distintos em função do valor inicial por litro de cada uma. Também fora avaliado o custo específico e o consumo específico de cada um dos biodieseis, a fim de determinar a diferença em relação ao óleo diesel comercial. No estudo de caso, os resultados mostraram vantagens para o óleo diesel, tanto no custo quanto no consumo. Comparando-se os biodieseis, o de sebo bovino apresentou-se com o menor custo de produção e o menor consumo.

Preliminary study of a methodology based on the degree-days concept for predicting the phenological phases of crops

This work develops a methodology (using the degree-days concept and linear regression), to forecast the duration of phenological phases in crops. An experiment was conducted in the greenhouse with three cultivars of cowpea (Vigna unguiculata (C.) Walp.), cv. California-781, Tvx 5058-09C and IT 81D-1032. The methodology was based on the relative thermal efficiency rate, determined for each species or cv. The results show that the proposed methodology may be a good alternative in works involving crops, especially because it does not require the repetition of the experiments.

Fracture strength of bovine incisors after intra-radicular treatment with MTA in an experimental immature tooth model

Aim To evaluate, using an experimental immature tooth model, the fracture resistance of bovine incisors submitted to different reinforcement treatments with mineral trioxide aggregate (MTA).Methodology An immature tooth model was created by sectioning the coronal and apical portions of 40 bovine incisors 8 mm above and 12 mm below the cementoenamel junction. The root canals were irrigated with 1.0% sodium hypochlorite. They were enlarged both coronally and apically using number 703 carbide burs (ISO: 500-104-168-007-021) and their internal diameter was standardized to 2.1 mm. The specimens were assigned to four groups (n = 10): GI-control (without filling); GII-apical MTA plug + filling with gutta-percha and endodontic sealer; GIII-filling with MTA; GIV-apical MTA plug + filling with MTA + metallic post (Reforpost I). A polyether impression material was used to simulate the periodontal ligament. The specimens were submitted to a compressive load at a crosshead speed of 0.5 mm min(-1) in a servo-hydraulic universal testing machine (MTS 810) applied at 45 degrees to the long axis of the tooth until failure. Data were submitted to statistical analysis by the Kruskal-Wallis test at 5% significance level.Results GIV presented the highest fracture resistance (32.7N) and differed significantly from the other groups (P < 0.05). No statistically difference was found between GII (16.6N) and GIII (23.4N) (P > 0.05). GIII had a significantly higher fracture resistance than GI (P < 0.05).Conclusions the use of MTA + metallic post as an intra-radicular reinforcement treatment increased the resistance to fracture of weakened bovine teeth in an experimental immature tooth model.

Influence of surgical repositioning of mature permanent dog teeth following experimental intrusion: a histologic assessment

The aim of this study was to evaluate, through histologic examination, the effect of surgical repositioning of intruded dog teeth upon the pulpal and surrounding tissues. Thirty teeth in 10 adult dogs, aged 2-3 years, were used. Fifteen teeth were intruded, surgically repositioned and fixed using orthodontics wire, composite resin, and enamel acid conditioning. All these teeth served as the experimental group. The remaining intruded teeth were not treated ( control group). The animals were sacrificed to allow observations at 7,15, and 30 post-operative days. The maxillary and mandibular archs were removed and processed for histologic exam. Based on the methodology and observed results, we concluded that: pulpal necrosis, external root resorption and ankylosis were common sequelae to severe traumatic intrusion; a careful immediate surgical repositioning of severed intruded permanent tooth with complete root formation has many advantages with few disadvantages.

Flammability limits: A review with emphasis on ethanol for aeronautical applications and description of the experimental procedure

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