Preparative separation and purification of bufadienolides from ChanSu by high-speed counter-current chromatography combined with preparative HPLC

Eight bufadienolides were successfully isolated and purified from ChanSu by high-speed counter-current chromatography (HSCCC) combined with preparative HPLC (prep-HPLC). First, a stepwise elution mode of HSCCC with the solvent system composed of petroleum ether - ethyl acetate - methanol - water (4:6:4:6, 4:6:5:5, v/v) was employed and four bufadienolides, two partially purified fractions were obtained from 200 mg of crude extract. The partially purified fractions III and VI were then further separated by prep-HPLC, respectively, and another four bufadienolides were recovered. Their structures were confirmed by ESI-MS and ¹H-NMR spectra.

Preparative separation of polyphenols from artichoke by polyamide column chromatography and high-speed counter-current chromatography

An efficient method for the rapid separation and purification of polyphenols from artichoke by polyamide column chromatography in combination with high-speed counter-current chromatography (HSCCC) was successfully built. The crude ethanol extracts from dry artichoke were first pre-separated by polyamide column chromatography and divided in two parts as sample 1 and sample 2. Then, the samples were further separated by HSCCC and yielded 7.8 mg of chlorogenic acid (compound I), 24.5 mg of luteolin-7-O-β-D-rutinoside (compound II), 18.4 mg of luteolin-7-O-β-D-glucoside (compound III), and 33.4 mg of cynarin (compound IV) with purity levels of 92.0%, 98.2%, 98.5%, and 98.0%, respectively, as determined by high-performance liquid chromatography (HPLC) method. The chemical structures of these compounds were identified by electrospray ionization-mass spectrometry (ESI-MS) and nuclear magnetic resonance (NMR).

Separation and purification of three stilbenes from the radix of Polygonum cillinerve (Nakai) Ohwl by macroporous resin column chromatography combined with high-speed counter-current chromatography

An effective method for the rapid separation and purification of three stilbenes from the radix of Polygonum cillinerve (Nakai) Ohwl by macroporous resin column chromatography combined with high-speed counter-current chromatography (HSCCC) was successfully established. In the present study, a two-phase solvent system composed of chloroform-n-butanol-methanol-water (4:1:4:2, v/v/v/v) was used for HSCCC separation. A one-step separation in 4 h from 150 mg of crude extract produced 26.3 mg of trans-resveratrol-3-O-glucoside, 42.0 mg of pieceid-2"-O-gallate, and 17.9 mg of trans-resveratrol with purities of 99.1%, 97.8%, and 99.4%, respectively, as determined by high-performance liquid chromatography (HPLC). The chemical structures of these compounds were identified by nuclear magnetic resonance (NMR) spectroscopy.

ENCAPSULAÇÃO DO ÁCIDO L-ASCÓRBICO NO BIOPOLÍMERO NATURAL GALACTOMANANA POR SPRAY‑DRYING: PREPARAÇÃO, CARACTERIZAÇÃO E ATIVIDADE ANTIOXIDANTE

AbstractIn this study, the spray drying technique was used to prepare L-ascorbic acid (AA) microparticles encapsulated with galactomannan-an extract from the seeds of the Delonix regia species. The physico-chemical characteristics, antioxidant activity, and encapsulation efficiency of the AA microparticles were evaluated and characterized using thermogravimetric analysis, differential scanning calorimetry, infrared spectroscopy, X-ray diffraction, and scanning electron microscopy. The free-radical scavenging activity of the AA microparticles was determined at different environmental conditions using DPPH (1,1-diphenyl-2-picryl-hydrazyl). X-ray diffraction measurements demonstrated a loss of crystallinity in AA after the encapsulation process, and a DSC scan also showed the loss of the compound's melting peak. Thermogravimetric analysis showed small differences in the thermal stability of galactomannan before and after the incorporation of AA. The mean diameters of the obtained spherical microspheres were in the range of 1.39 ± 0.77 µm. The encapsulation efficiency of AA microparticles in different environmental conditions varied from 95.40 to 97.92, and the antioxidant activity showed values ranging from 0.487 to 0.550 mg mL-1.

COMPARISON BETWEEN WOOD DRYING DEFECT SCORES: SPECIMEN TESTING X ANALYSIS OF KILN-DRIED BOARDS

It is important to develop drying technologies for Eucalyptus grandis lumber, which is one of the most planted species of this genus in Brazil and plays an important role as raw material for the wood industry. The general aim of this work was to assess the conventional kiln drying of juvenile wood of three clones of Eucalyptus grandis. The specific aims were to compare the behavior between: i) drying defects indicated by tests with wood specimens and conventional kiln-dried boards; and ii) physical properties and the drying quality. Five 11-year-old trees of each clone were felled, and only flatsawn boards of the first log were used. Basic density and total shrinkage were determined, and the drying test with wood specimens at 100 °C was carried out. Kiln drying of boards was performed, and initial and final moisture content, moisture gradient in thickness, drying stresses and drying defects were assessed. The defect scoring method was used to verify the behavior between the defects detected by specimen testing and the defects detected in kiln-dried boards. As main results, the drying schedule was too severe for the wood, resulting in a high level of boards with defects. The behavior between the defects in the drying test with specimens and the defects of kiln-dried boards was different, there was no correspondence, according to the defect scoring method.

Mathematical models to describe the volumetric shrinkage rate of red beans during drying

The present study aimed to determine the volumetric shrinkage rate of bean (Phaseolus vulgaris L.) seeds during air-drying under different conditions of air, temperature and relative humidity, and to adjust several mathematical models to the empiric values observed, and select the one that best represents the phenomenon. Six mathematical models were adjusted to the experimental values to represent the phenomenon. It was determined the degree of adjustment of each model from the value of the coefficient of determination, the behavior of the distribution of the residuals, and the magnitude of the average relative and estimated errors. The rate of volumetric shrinkage that occurred in bean seeds during drying is between 25 and 37%. It basically depends on the final moisture content, regardless of the air conditions during drying. The Modified Bala & Woods' model best represented the process.

Application of simulated annealing in simulation and optimization of drying process of Zea mays malt

Kinetic simulation and drying process optimization of corn malt by Simulated Annealing (SA) for estimation of temperature and time parameters in order to preserve maximum amylase activity in the obtained product are presented here. Germinated corn seeds were dried at 54-76 °C in a convective dryer, with occasional measurement of moisture content and enzymatic activity. The experimental data obtained were submitted to modeling. Simulation and optimization of the drying process were made by using the SA method, a randomized improvement algorithm, analogous to the simulated annealing process. Results showed that seeds were best dried between 3h and 5h. Among the models used in this work, the kinetic model of water diffusion into corn seeds showed the best fitting. Drying temperature and time showed a square influence on the enzymatic activity. Optimization through SA showed the best condition at 54 ºC and between 5.6h and 6.4h of drying. Values of specific activity in the corn malt were found between 5.26±0.06 SKB/mg and 15.69±0,10% of remaining moisture.

Solar drying of jack fruit almonds

Dryers heated by solar energy have been constructed and used in drying whole and half jack fruit almonds. The samples were dried during the day in direct sun and in the conventional solar dryer prepared for this purpose. Another piece of equipment was built for reception and accumulation of sun energy in a body of water, which was used as a heat source for night drying. The drying with the sun energy was compared with artificial drying. The jack fruit almonds were dried whole, half, with pellicle and without it. The storage of solar energy in water was technically viable for use in night drying. The drying by combining solar dryers in the day and night periods were completed in approximately 35 hours, and were equivalent to artificial drying between 40ºC and 70ºC. Almond cut in half and the pellicle removed reduced the drying time.

Effective diffusivity and convective mass transfer coefficient during the drying of bananas

In this article, a methodology is used for the simultaneous determination of the effective diffusivity and the convective mass transfer coefficient in porous solids, which can be considered as an infinite cylinder during drying. Two models are used for optimization and drying simulation: model 1 (constant volume and diffusivity, with equilibrium boundary condition), and model 2 (constant volume and diffusivity with convective boundary condition). Optimization algorithms based on the inverse method were coupled to the analytical solutions, and these solutions can be adjusted to experimental data of the drying kinetics. An application of optimization methodology was made to describe the drying kinetics of whole bananas, using experimental data available in the literature. The statistical indicators enable to affirm that the solution of diffusion equation with convective boundary condition generates results superior than those with the equilibrium boundary condition.

Performance of spray nozzles in land applications with high speed

The aim of this study was to evaluate different spray nozzles for land applications in high speed on the coverage and deposit in soybean plants pulverization. It was evaluated the AXI 110 04 plane jet nozzles operated at speed of 4.17m.s-1 (control), the grey APE and the AXI 110 08 plane jets, and the TD HiSpeed 110 06 and AXI TWIN 120 06 twin jets, at speed of 9.72m.s-1. The application volume was fixed in 120L ha-1. The application efficiency was evaluated by two different methods: analysis of the coverage area using fluorescent pigment and UV light and analysis of deposits through the recovery and quantification of FD&C N°1 brilliant blue marker by spectrophotometry. Both analyses were done in samples collected from top, middle and bottom parts of the plants. The spray nozzles showed differences in coverage and deposit pattern, so in the top part, the coverage was increased with smaller drops and the deposits were increased with medium drops. In the other parts of the plants, there were no statistical differences between the treatments for both coverage and deposits. The displacement speed did not influence the application efficiency for nozzles with the same drop pattern, and the obtained spray coverage and deposits at the medium and bottom parts of the plants were less than 50% of that found at the top of the soybean plants.

Adaptation of "Niagara Rosada" grape must to winemaking by partial cluster dehydration

This study aimed to verify the influence of partial dehydration of "Niagara Rosada" grape clusters in physicochemical quality of the pre- fermentation must. In Brazil, during the winemaking process it is common to need to adjust the grape must when the physicochemical characteristics of the raw material are insufficient to produce wines in accordance with the Brazilian legislation for classification of beverages, which establishes the minimum alcohol content of 8.6 % for the beverage to be considered wine. Therefore, given that the reduction in the water content of grape berries allows the concentration of chemical compounds present in its composition, especially the concentration of total soluble solids, we proceeded with the treatments that were formed by the combination of two temperatures (T1-37.1ºC and T2-22.9 ºC) two air speeds (S1: 1.79 m s-1 and S2: 3.21 m s-1) and a control (T0) that has not gone through the dehydration treatment. Analysis of pH, Total Titratable Acidity (TTA) were performed in mEq L-1, Total Soluble Solids (TSS) in ºBrix, water content on a dry basis and Concentration of Phenolic Compounds (CPC) in mg of gallic acid per 100g of must. The average comparison test identified statistically significant modifications for the adaptation of must for winemaking purposes, having the treatment with 22.9 ºC and air speed of 1.79 m s-1 shown the largest increase in the concentration of total soluble solids, followed by the second best result for concentration of phenolic compounds.

Mechanical properties of castor beans subject to different drying temperatures aiming to disrupt the bean coat

In castor oil extraction process, the bean coat is abrasive to the equipment and releases substances that modify the oil color, reducing its quality. A potential solution would be to run the extraction by compressing only the endosperm. Due to lack of information, the objective of this study was to evaluate the influence of forced air drying at 40, 60, 80 and 100 ºC and farmyard drying, in the mechanical properties of the beans, aiming to break the bean coat. Castor beans were subjected to compression tests, in two perpendicular directions, at a strain rate of 0.6 mm.s-1. Average values of force, deformation energy, strain, all at rupture, and stiffness were used to evaluate the effects of dehydration. It was observed that the heat treatments did not alter the mechanical properties of castor beans, the strain and stiffness values discriminate the differences between the directions and had the lowest coefficients of variation. It was concluded that forced air drying, more costly than farmyard drying, does not bring benefits to the decortication. However, regardless the heat treatment used, the mechanical stress lengthwise is the most suitable to promote decortication.

Determination of physical properties of crambe fruits during drying

The Knowledge of the physical properties of agricultural products has great importance for the construction and operation of equipment for drying and storage, to achieve increased efficiency in post-harvest operations. The aim was to determine and analyze the physical properties of crambe fruits during drying at different temperatures. Crambe fruits with an initial moisture content of 0.36 (decimal d.b.) which was reduced by drying at 37.0; 58.8 and 83.5 ºC and relative humidity of 29.4; 11.2 and 3.2%, respectively, to 0.09 ± 1 (decimal d.b.). At different levels of moisture contents (0.36; 0.31; 0.26; 0.21; 0.17; 0.13 and 0.09 decimal d.b.), was evaluated the intergranular porosity, the bulk density, the true density as well as the volumetric shrinkage and the fruit mass. The study was installed by the factorial 3 x 7, and three drying temperatures and seven moisture contents in a randomized design. Data were analyzed using regression. The bulk density and the true density decreases along the drying process; the volumetric shrinkage and the mass increased with lower moisture content and the intergranular porosity decreased sharply with the increasing drying temperature.

Microencapsulation of pequi pulp by spray drying: use of modified starches as encapsulating agent

The aim of this study was to evaluate the microencapsulation of pequi pulp by spray drying. A central composite rotational design was used in order to evaluate the effect of the independent variables: inlet air temperature, surfactant concentration and modified starch concentration. The dependent variables were assumed as yield of the process and the product features microencapsulated. A selection of the best process condition was performed to obtain the best condition of a product with the highest vitamin C and carotenoids content. Powders showed moisture content below 2%. The experimental values of hygroscopicity, yield, water activity, total carotenoids and vitamin C powders ranged from 7.96 to 10.67 g of adsorbed water/100g of solids, 24.34 to 49.80%, 0.13 to 0.30, 145.78 to 292.11 mg of ascorbic acid/g of pequi solids and 15.51 to 123.42 mg of carotenoids/g of pequi solids, respectively. The inlet air temperature 140°C, the surfactant concentration of 2.5% and the modified starch concentration of 22.5% was recommended as the selected condition. By the scanning electron microscopy, it was observed that most of the particles had spherical shape and smooth surface.

Mathematical simulation parameters for drying of cassava starch pellets

Based on experimental tests, it was obtained the equations for drying, equilibrium moisture content, latent heat of vaporization of water contained in the product and the equation of specific heat of cassava starch pellets, essential parameters for realizing modeling and mathematical simulation of mechanical drying of cassava starch for a new technique proposed, consisting of preformed by pelleting and subsequent artificial drying of starch pellets. Drying tests were conducted in an experimental chamber by varying the air temperature, relative humidity, air velocity and product load. The specific heat of starch was determined by differential scanning calorimetry. The generated equations were validated through regression analysis, finding an appropriate correlation of the data, which indicates that by using these equations, can accurately model and simulate the drying process of cassava starch pellets.