Determinação de etanol e voláteis relacionados em sangue e fluido oral por microextração em fase sólida em headspace associada à cromatografia gasosa com detector de ionização em chama

The aim of this study was to validate a method for the determination of acethaldehyde, methanol, ethanol, acetone and isopropanol employing solid-phase microextraction associated to gas chromatography with flame ionization detection. The operational conditions of SPME were optimized by response surface analysis. The calibration curves for all compounds were linear with r² > 0.9973. Accuracy (89.1-109.0%), intra-assay precision (1.8-8.5%) and inter-assay precision (2.2-8.2%) were acceptable. The quantification limit was 50 µg/mL. The method was applied to the meaurement of ethanol in blood and oral fluid of a group of volunteers. Oral fluid ethanol concentrations were not directly correlated with blood concentrations.

Optimization of solvent mixtures for extraction from bark of Schinus terebinthifolius by a statistical mixture-design technique and development of a UV-Vis spectrophotometric method for analysis of total polyphenols in the extract

A statistical mixture-design technique was used to study the effects of different solvents and their mixtures on the yield, total polyphenol content, and antioxidant capacity of the crude extracts from the bark of Schinus terebinthifolius Raddi (Anacardiaceae). The experimental results and their response-surface models showed that ternary mixtures with equal portions of all the three solvents (water, ethanol and acetone) were better than the binary mixtures in generating crude extracts with the highest yield (22.04 ± 0.48%), total polyphenol content (29.39 ± 0.39%), and antioxidant capacity (6.38 ± 0.21). An analytical method was developed and validated for the determination of total polyphenols in the extracts. Optimal conditions for the various parameters in this analytical method, namely, the time for the chromophoric reaction to stabilize, wavelength of the absorption maxima to be monitored, the reference standard and the concentration of sodium carbonate were determined to be 5 min, 780 nm, pyrogallol, and 14.06% w v-1, respectively. UV-Vis spectrophotometric monitoring of the reaction under these conditions proved the method to be linear, specific, precise, accurate, reproducible, robust, and easy to perform.

Experimento didático de quimiometria para planejamento de experimentos: avaliação das condições experimentais na determinação espectrofotométrica de ferro II com o-fenantrolina. Um tutorial, parte III

The objective of this manuscript is to describe a practical experiment that can be employed for teaching concepts related to design of experiments using Matlab or Octave computing environment to beginners, undergraduate and graduate students. The classical experiment for determination of Fe (II) using o-phenanthroline was selected because it is easy to understand, and all the required materials are readily available in most analytical laboratories. The approach used in this tutorial is divided in two steps: first, the students are introduced to the concept of multivariate effects, how to calculate and interpret them, and the construction and evaluation of a linear model to describe the experimental domain by using a 2³ factorial design. Second, an extension of the factorial design by adding axial points is described, thereby, providing a central composite design. The quadratic model is then introduced and used to build the response surface.

OTIMIZAÇÃO DO PROCESSO DE TRANSESTERIFICAÇÃO EM DUAS ETAPAS PARA PRODUÇÃO DE BIODIESEL ATRAVÉS DO PLANEJAMENTO EXPERIMENTAL DOEHLERT

In this work, Doehlert experimental design was used to optimize the Transesterification Double Step Process (TDSP) method of methyl soybean oil biodiesel production which starts with a basic catalysis followed by an acidic catalysis. The conversion values were calculated from NMR spectra. Response surface was used to show the results of the interactions between the variables. This experimental design evaluated variables like catalyst and alcohol amount for the basic catalysis and time and temperature for the acidic catalysis. According to results obtained after Doehlert design application the alcohol amount was the main factor that influenced on the basic catalysis but for the acidic catalysis both time and temperature are important and their effects are opposite. It resulted on excellent conversions for both steps obtaining for the basic catalysis about 100% when was used like optimal conditions catalyst amount equal to 0.40 g and volume of methanol equal to 60 mL and for the acidic catalysis about 99% when was used like optimal conditions temperature of 65 °C and 90 minutes for reaction time.

Influence of temperature and leaf wetness duration in the severity of Cercospora leaf spot of beet

ABSTRACT In the present study, the influence of temperature (15, 20, 25, 30 and 35°C) and leaf wetness period (6, 12, 24 and 48 hours) on the severity of Cercospora leaf spot of beet, caused by Cercospora beticola, was studied under controlled conditions. Lesion density was influenced by temperature and leaf wetness duration (P<0.05). Data were subjected to nonlinear regression analysis. The generalized beta function was used for fitting the disease severity and temperature data, while a logistic function was chosen to represent the effect of leaf wetness on the severity of Cercospora leaf spot. The response surface resultant of the product of the two functions was expressed as ES = 0.0001105 * (((x-8)2.294387) * ((36-x)0.955017)) * (0.39219/(1+25.93072 * exp (-0.16704*y))), where: ES represents the estimated severity value (0.1); x, the temperature (ºC) and y, the leaf wetness duration (hours). This model should be validated under field conditions to assess its use as a computational forecast system for Cercospora leaf spot of beet.

Development of a weather-based model for Botrytis leaf blight of onion

ABSTRACT In the present study, onion plants were tested under controlled conditions for the development of a climate model based on the influence of temperature (10, 15, 20 and 25°C) and leaf wetness duration (6, 12, 24 and 48 hours) on the severity of Botrytis leaf blight of onion caused by Botrytis squamosa. The relative lesion density was influenced by temperature and leaf wetness duration (P <0.05). The disease was most severe at 20°C. Data were subjected to nonlinear regression analysis. Beta generalized function was used to adjust severity and temperature data, while a logistic function was chosen to represent the effect of leaf wetness on the severity of Botrytis leaf blight. The response surface obtained by the product of two functions was expressed as ES = 0.008192 * (((x-5)1.01089) * ((30-x)1.19052)) * (0.33859/(1+3.77989 * exp (-0.10923*y))), where ES represents the estimated severity value (0.1); x, the temperature (°C); and y, the leaf wetness (in hours). This climate model should be validated under field conditions to verify its use as a computational system for the forecasting of Botrytis leaf blight in onion.

Production of natural aroma by yeast in wastewater of cassava starch industry

ABSTRACT2-Phenylethanol (PE) is an aromatic alcohol with a characteristic odor of roses, widely used in food industry to modify certain aroma compositions in formulations with fruit, jam, pudding, and chewing gums, and also in cosmetic and fragrance industry. This compound occurs naturally in low concentrations in some essential oils from flowers and plants. An alternative to plants extraction are biotechnological processes. This study evaluated 2-phenylethanol’s production in cultivation of Saccharomyces cerevisiae in cassava wastewater originated from starch industry. The substrate was supplemented with glucose and L-phenylalanine in order to obtain higher 2-phenylethanol concentrations and better efficiency in glucose/2-phenylethanol conversion. It was performed using Rotatable Center Composite Design and response surface analysis. Cultures were performed under aerobic conditions in a batch system in Erlenmeyer flasks containing 50 mL of medium in shaker at 150 rpm and 24 ± 1 ºC. The highest PE values ​​were obtained with supplementation of 20.0 g.L-1 of glucose and 5.5 g.L-1 of L-phenylalanine, which has been experimentally validated, obtaining a PE production of 1.33 g.L-1 and PE/glucose yield factor of 0.070 g.g-1, equivalent to 74.3 and 89.7% ​​of desirability values according to the validated model.

Herbicide efficacy on Borreria densiflora control in pre- and post-emergence conditions

The weed Borreria densiflora is a management issue in soybean and sugarcane crops from North and Northeastern Brazil. Knowledge upon chemical control of B. densiflora contributes to the integrated management of this weed species, especially when active ingredient options become reduced due to the selection of herbicide resistant or tolerant weed species. Experiments in pre- and post-emergence of B. densiflora were conducted in greenhouse, in a randomized block design and four replications. In pre-emergence, the dose-response curve methodology was used and 7 herbicides were tested. In post-emergence, 9 herbicides at the recommended rate and 4 herbicide mixtures were tested. For pre and post-emergence conditions, evaluations were conducted at 60 and 21 days after treatment (DAT), respectively, and the variables analyzed were weed control and dry weight (%). The results showed options of pre-emergent herbicides that can be used for controlling B. densiflora, especially in sugarcane, where chemical weed control is mainly based on pre-emergent applications. In the current glyphosate resistance scenario, one should consider the use of pre-emergent herbicides within an integrated management of B. densiflora. For satisfactory post-emergence control, B. densiflora plants should be sprayed at the phenological stage of up to three pairs of leaves. Herbicide mixtures have been and will continue to be an important tool in chemical weed management, broadening the spectrum of weed control, while diversifying herbicide mechanisms of action, which helps to prevent or delay the appearance of herbicide resistance.

Development and chemical characterization of flour obtained from the external mesocarp of "pequizeiro" fruit

The objective of this work was to develop a recommendation for the chemical peeling of pequi fruit and characterize the flour obtained from the external mesocarp of "Pequizeiro", pequi tree (Caryocar brasiliense Camb.). The technology applied to obtain the external mesocarp pequi flour included the epicarp removal with NaOH solution. The Response Surface Method was used to optimize the chemical peeling process by applying the Central Composite Rotatable Design, with eleven trials including three replicates at the central point, varying the NaOH aqueous solution concentration and fruit immersion time. The mass loss was evaluated through the analysis of variance and using bi and three dimensional graphs. The chemical characteristics of the external mesocarp pequi flour evaluated were: moisture content, ashes, proteins, lipids, total carbohydrates, dietary fiber, and some minerals. The best combination for an efficient removal of the fruit peel with the lowest mass loss was reached with 7.05 minutes of immersion in a 5.08 g.L-1 NaOH aqueous solution. This study indicated that the external mesocarp pequi flour is a food source rich in dietary fiber, carbohydrates, ashes, magnesium, calcium, manganese, and copper, but it is poor in lipids, zinc, and iron.

Docosahexaenoic acid ethyl esther (DHAEE) microcapsule production by spray-drying: optimization by experimental design

Docosahexaenoic acid is an essential polyunsaturated fatty acid with important metabolic activities. Its conjugated double bonds make it susceptible to decomposition. Its stability may be improved through fatty acid entrapment with a spray-drying technique; however, the many parameters involved in this technique must be considered to avoid affecting the final product quality. Therefore, this study aimed to evaluate the entrapment conditions and yields of fish oil enriched with docosahexaenoic acid ethyl ester. Microcapsules were obtained from Acacia gum using a spray-drying technique. The experimental samples were analyzed by chromatography and delineated by Statistica software, which found the following optimum entrapment conditions: an inlet temperature of 188 °C; 30% core material; an N2 flow rate of 55 mm; and a pump flow rate of 12.5 mL/minute. These conditions provided a 66% yield of docosahexaenoic acid ethyl ester in the oil, corresponding to 19.8% of entrapped docosahexaenoic acid ethyl ester (w/w). This result was considered significant since 30% corresponded to wall material.

Kinetic, thermodynamic properties, and optimization of barley hydration

The hydration kinetics of five barley cultivars was studied at six different temperatures ranging from 10 to 35 ºC for 32 hours applying the Peleg model. Response Surface was used to describe dynamic of the process and identify the hydration time for each cultivar. The activation energy (Ea), enthalpy (ΔH*), entropy (ΔS*), and Gibbs free energy (ΔG*) were estimated from the adjusted parameters and Arrhenius equation. Temperature had significant effect on the hydration of the five cultivars. At low temperatures, the stabilization time for hydration was faster. Peleg constants K1 and K2 decreased with increasing temperature. The cultivar BRS BRAU showed the lowest value of initial absorption rate (R0 = 0.149 kg.h-1) at 10 ºC, while the cultivar BRS BOREMA had the highest value of R0 (0.367 kg.h-1 at 35 ºC). The equilibrium moisture content (Me) increased with increasing temperature. The cultivars BRS CAUE and BRS BRAU showed the lowest values of Ea, ΔH*, ΔS* showed negative values, and ΔG* increased with increasing temperature, confirming the effect of temperature on hydration.

Microencapsulation of babassu coconut milk

The objective of this study was to obtain babassu coconut milk powder microencapsulated by spray drying process using gum Arabic as wall material. Coconut milk was extracted by babassu peeling, grinding (with two parts of water), and vacuum filtration. The milk was pasteurized at 85 ºC for 15 minutes and homogenized to break up the fat globules, rendering the milk a uniform consistency. A central composite rotatable design with a range of independent variables was used: inlet air temperature in the dryer (170-220 ºC) and gum Arabic concentration (10-20%, w/w) on the responses: moisture content (0.52-2.39%), hygroscopicity (6.98-9.86 g adsorbed water/100g solids), water activity (0.14-0.58), lipid oxidation (0.012-0.064 meq peroxide/kg oil), and process yield (20.33-30.19%). All variables influenced significantly the responses evaluated. Microencapsulation was optimized for maximum process yield and minimal lipid oxidation. The coconut milk powder obtained at optimum conditions was characterized in terms of morphology, particle size distribution, bulk and absolute density, porosity, and wettability.

Optimization of the HS-SPME-GC/MS technique for determining volatile compounds in red wines made from Isabel grapes (Vitis labrusca)

Abstract Brazilian wine production is characterized by Vitis labrusca grape varieties, especially the economically important Isabel cultivar, with over 80% of its production destined for table wine production. The objective of this study was to optimize and validate the conditions for extracting volatile compounds from wine with the solid-phase microextraction technique, using the response surface method. Based on the response surface analysis, it can be concluded that the central point values maximize the process of extracting volatile compounds from wine, i.e., an equilibrium time of 15 minutes, an extraction time of 35 minutes, and an extraction temperature of 30 °C. Esters were the most numerous compounds found under these extraction conditions, indicating that wines made from Isabel cultivar grapes are characterized by compounds that confer a fruity aroma; this finding corroborates the scientific literature.

Merozoite surface protein 2 allelic variation influences the specific antibody response during acute malaria in individuals from a Brazilian endemic area

The antibody response to Plasmodium falciparum parasites of naturally infected population is critical to elucidate the role of polymorphic alleles in malaria. Thus, we evaluated the impact of antigenic diversity of repetitive and family dimorphic domains of the merozoite surface protein 2 (MSP-2) on immune response of 96 individuals living in Peixoto de Azevedo (MT-Brazil), by ELISA using recombinant MSP-2 proteins. The majority of these individuals were carrying FC27-type infections. IgG antibody responses were predominantly directed to FC27 parasites and were correlated to the extension of polymorphism presented by each MSP-2 region. This finding demonstrated the impact of the genetic polymorphism on antibody response and therefore, its importance on malaria vaccine efficacy.

Influence of carbon source and the fermentation process on levan production by Zymomonas mobilis analyzed by the surface response method

The aim of this study is to assess sugar cane juice and sucrose as substrates, the batch and fed batch processes and their interaction in the levan production using a complete factorial design. Zymomonas mobilis was cultivated in different sugar cane juice and sucrose concentrations in two fermentation processes at 25 °C for 20 h. A complete factorial design (2³) was used to analyze the effects of the type and concentration of the substrate, as well as the batch and fed batch processes. A complete second factorial design (2²) was used to observe the importance of sugar cane juice. The results indicated that the batch process improved the levan production reaching 40.14 g/L. The addition of sugar cane juice was not statistically significant for levan formation, however sugar cane juice stimulated biomass, sorbitol and ethanol production. The best medium for levan production was 150 g/L sucrose in batch.