Determinação rápida de fármacos básicos em plasma por cromatografia a gás com detector de nitrogênio e fósforo

A simple and fast method for determination of 40 basic drugs in human plasma employing gas-chromatography with nitrogen-phosphorus detection was developed and validated. Drugs were extracted from 800 µL of plasma with 250 µL of butyl acetate at basic pH. Aliquots of the organic extract were directly injected on a column with methylsilicone stationary phase. Total chromatographic run time was 25 min. All compounds were detected in concentrations ranging from therapeutic to toxic levels, with intermediate precision CV% below 11.2 and accuracy in the range of 92-114%.

Desenvolvimento e validação de método espectrofotométrico para determinação de corante à base de luteína adicionado em iogurte desnatado

A simple analytical method for extraction and quantification of lutein colorant added to yogurt was developed and validated. The method allowed complete extraction of carotenoids using tetrahydrofuran in vortex, followed by centrifugation, partition to diethyl ether/petroleum ether, and drying. The carotenoids dissolved in ethanol were quantified by UV-Vis spectrophotometry. This method showed linearity in the range tested (1.41-13.42 µg g-1), limits of detection and quantification of 0.42 and 1.28 µg g-1, respectively, low relative standard deviation (3.4%) and recovery ranging from 95 to 103%. The method proved reliable for quantification of lutein added to yogurt.

Guia para a determinação da estabilidade de produtos químicos

Companies worldwide are reviewing their working process to avoid waste, become aligned with environmental management standards and to fulfill specifications defined for national and international regulations. In this context, it is important that Brazilian Chemical companies have a specific stability guide for their products. The main purpose of this work is to present a stability guide for chemical products based on the existing guides of the Pharmaceutical and Cosmetics segments. Furthermore, this work proposes to offer an additional period of shelf life for chemical products, provided they meet certain prerequisites.

Determinação da difusividade efetiva de raiz de chicória

Inulin is a fructooligosacharide found in diverse agricultural products, amongst them garlic, banana, Jerusalem artichoke and chicory root. Inulin generally is used in developed countries, as a substitute of sugar and/or fat due to its characteristics of fitting as functional and dietary food. Chicory root is usually used as source and raw material for commercial extration of inulin. The experiments consisted on drying sliced chicory roots based on a factorial experimental design in a convective dryer whose alows the air to pass perpendicularly through the tray. Effective diffusivity (dependent variable) has been determined for each experimental combination of independent variables (air temperature and velocity). The data curves have been fitted by the solution of the second Fick law and Page's model. Effective difusivity varied from 3.51 x 10-10 m² s-1 to 1.036 x 10-10 m² s-1. It is concluded that, for the range of studied values, air temperature is the only statistically significant variable. So, a first order mathematical model was obtained, representing effective diffusivity behavior as function of air temperature. The best drying condition was correspondent to the trial using the highest drying air temperature.

Determinação em tempo real da magnitude de danos físicos por impacto em linhas de beneficiamento e em condições de laboratório e seus efeitos na qualidade de tomate

Tomatoes are one of the most important vegetable crops grown in Brazil and are among the crops that have one of the highest post-harvest losses indexes in the country. The present work aimed at evaluating impact damage observed in packing lines of fresh tomatoes as well as to determine, under laboratory conditions, quality alterations of tomato fruits submitted to impact damage in different surface types. Critical points evaluation was accomplished using an instrumented sphere. Critical transference points found showed variations in acceleration levels from 30 to 129 G (m s-2). Tests carried out under laboratory conditions showed that padded surfaces reduced up to 31% impact damage. Incidence of severe internal physical damage was evaluated by a subjective scale and increased by 79% on hard surfaces for the highest fall drop. On the other hand, it was observed an effective reduction in physical damage on fruits when padded surfaces were used. When a 10-cm drop was performed, the maximum reduction measured was 10% for hard surfaces and 5% for previously padded surfaces. For quality parameters, it was observed for high drops on hard surfaces, highest values for weight loss, total acidity, lower values for vitamin C and Soluble Solids.

Determinação do máximo déficit acumulado de oxigênio: efeito da duração dos testes submáximos para predição da demanda de oxigênio

The aim of this study was to investigate the influence of different assessment time periods of submaximal tests on the determination of the maximal accumulated oxygen deficit (MAOD), through the adoption of different time slots of 4 to 6, 6 to 8 and 8 to 10 min. Ten cyclists with mean age of 27.5 ± 4.1 years, body mass 74.4 ± 12.7 kg and time experience of 9.8 ± 4.7 years participated in this study. The athletes underwent an incremental exercise test to determine the peak oxygen consumption (VO2peak), and four submaximal constant work-load test sessions (60, 70, 80 and 90% VO2peak) of 10 min in order to estimate the O2 demand (DEO2). The mean VO2 values obtained on each constant work-load for the 4 to 6, 6 to 8 and 8 to 10 min time-periods intervals were used to perform a linear regression between the intensity and O2 consumption for each time-period. In addition, the subjects performed one supramaximal rectangular test (110% VO2peak) for the quantification of MAOD. There was no significant difference in VO2 between the different time-periods for all submaximal tests (P> 0.05). Similarly, no significant difference was found in DEAO2 and MAOD (P> 0.05). Furthermore, the values of MAOD for the three time-periods intervals showed good agreement and strong correlation. Thus, the data suggest that the submaximal tests used to estimate the values of MAOD can be reduced, at least in this type of sample, and with the use of a cycle simulator.

Determinação de substitutos da manteiga de cacau em coberturas de chocolate através da análise de triacilgliceróis

Brazilian regulations prohibit the addition of cocoa butter replacements to chocolate, in total or partial substitution. The objective of the present work was to check the quality standards of four of coating bitter Brasilian chocolate bars and five of coating milk chocolate bars, commercialized in Campinas. In order to check the possible addition of substitutes, the triacylglycerol composition was determined, and the results were analysed by Padley & Timms mathematical method. The triacylglycerol composition of each sample was determined by high temperature gas chromatography (HTGC). The presence of cocoa butter replacements was not detected in the brands of coating chocolate.

Determinação da velolcidade critica como referencia do limiar anaerobio para o nado costas

Universidade Estadual de Campinas . Faculdade de Educação Física

Comparação entre protocolos de determinação do limiar anaerobio e suas correlações com o desempenho aerobio em nadadores adolescentes

Universidade Estadual de Campinas . Faculdade de Educação Física

Metodologia para determinação dos volumes do tronco durante a respiração usando projeção de luz e reconstrução de superficie

Universidade Estadual de Campinas . Faculdade de Educação Física

Determinação de aflatoxina B1 em rações e aflatoxina M1 no leite de propriedades do Estado de São Paulo

A ocorrência de aflatoxina B1 (AFB1) em rações e aflatoxina M1 (AFM1) no leite cru foi avaliada em propriedades leiteiras situadas na região nordeste do Estado de São Paulo, Brasil, de outubro de 2005 a fevereiro de 2006. A análise de aflatoxinas foi efetuada utilizando-se colunas de imunoafinidade para purificação dos extratos, sendo a quantificação realizada através de cromatografia líquida de alta eficiência. A AFB1 foi detectada em 40% das rações em níveis de 1,0 a 19,5 μg.kg-1. A concentração de AFM1 em 36,7% de amostras de leite positivas variou de 0,010 a 0,645 μg.L-1. Somente uma amostra de leite estava acima do limite de tolerância adotado no Brasil (0,5 μg.L-1) para AFM1. Concluiu-se que as concentrações de aflatoxinas na ração e no leite foram relativamente baixas, embora a alta frequência das aflatoxinas nas amostras analisadas indique a necessidade de contínuo monitoramento a fim de prevenir a contaminação de ingredientes e rações destinadas ao gado leiteiro.

Comparação de técnicas de determinação de ésteres em cachaça

An analytical comparison of three different techniques for quantitative profile of esters in cachaça is reported. The Ministério da Agricultura Pecuária e Abastecimento (MAPA) recommends the use of GC/FID or volumetry. Despite being laborious and lacking in chemical speciation, the volumetric technique for total ester content shows to be appropriate, reproducible, and accurate for the analysis of cachaça. However, the GC/FID suggested by MAPA, considering only ethyl acetate, shows inaccuracy, underestimating the total ester content by a median factor of 72%, mainly due to the absence of ethyl lactate analysis. On the other hand, the GC/MS technique that comprises the analysis and speciation of nine esters, including ethyl lactate, proved to be reproducible, simple, fast and accurate for the analysis of total ester content in cachaça. Thus, the total ester content results obtained using GC/FID must be considered with precaution.

Hidrólise do óleo de Azadirachta indica em água subcrítica e determinação da composição dos triacilglicerídeos e ácidos graxos por cromatografia gasosa de alta resolução a alta temperatura e cromatografia gasosa de alta resolução acoplada à espectrometria de massas

The development of modern analytical tools plays an important role in quality control. The main purpose of this study was to explore the use of subcritical water as a versatile analytical tool, employed simultaneously as a reagent and solvent, as well as the application of high temperature-high resolution gas chromatography (HT-HRGC) to develop a procedure for the analysis of triacylglycerides and fatty acids in Azadirachta indica A. Juss. (Neem) oil without the need for solvents, chemical reagents, or catalytic agents. The developed method presented satisfactory results and is in agreement with the concepts of Green Analytical Chemistry (GAC).

Avaliação de solventes de extração por ultrassom usando-se cromatografia líquida de alta eficiência para a determinação de hidrocarbonetos policíclicos aromáticos em solos contaminados

A method using ultrasonication extraction for the determination of 17 polycyclic aromatic hydrocarbons (PAHs), selected by the USEPA and NIOSH as "consent decree" priority pollutants, in soil by High Performance Liquid Chromatography (HPLC) was studied. Separation and detection were completed in 20 min with a C18 columm, acetonitrile-water gradient elution and ultraviolet absorption and fluorescence detections. The detection limits, for a 10 µL of solution injection, were less than 9,917 ng/g in UV detection and less than 1,866 ng/g in fluorescence detection. Several organic solvents were tested for extraction of the 17 PAHs from soils. Acetone was the best solvent among the three solvents tested, and the order of the extraction efficiencies was: acetone>methanol>acetonitrile. Ultrasonication using acetone as solvent extraction was used to evaluate the biodegradation of those compounds in contaminated soil during a vermicomposting process.

Determinação espectrométrica dos flavonóides das folhas de Maytenus (Celastraceae) e de Passiflora (Passifloraceae) e comparação com método CLAE-UV

Este trabalho apresenta uma modificação dos procedimentos descritos nas Farmacopéias Francesa e Européia para a análise de flavonoides de Passiflora incarnata L., Passifloraceae, por espectrometria UV-Visível e propõe a sua aplicação na determinação dos flavonoides totais das folhas da espinheira-santa (Maytenus aquifolium Mart. e Maytenus ilicifolia (Schrad.) Planch., Celastraceae) e do maracujá (Passiflora edulis Sims. e Passiflora alata Curtis, Passifloraceae). Os resultados obtidos por espectrometria no UV-Visível foram comparados aos obtidos por cromatografia líquida de alta eficiência (CLAE-UV), encontrando-se resultados estatisticamente similares entre os métodos espectrométrico modificado da Farmacopéia Francesa e CLAE-UV.