Synthesis of quinoxaline 1,4-di-N-oxide derivatives on solid support using room temperature and microwave-assisted solvent-free procedures

We describe the synthesis of 12 new ethyl and methyl quinoxaline-7-carboxylate 1,4-di-N-oxide derivatives on solid supports with room temperature and microwave-assisted solvent-free procedures. Results show that solid supports have good catalytic activity in the formation of quinoxaline 1,4-di-N-oxide derivatives. We found that florisil and montmorillonite KSF and K10 could be used as new, easily available, inexpensive alternatives of catalysts. Additionally, room temperature and microwave-irradiation solvent-free synthesis was more efficient than a conventional procedure (Beirut reaction), reducing reaction time and increasing yield.

Use of heterogeneous catalysts in methylic biodiesel production induced by microwave irradiation

The effect of different heterogeneous catalysts on the microwave-assisted transesterification of sunflower oil for the production of methylic biodiesel in a monomode microwave reactor is described. The experiments were carried out at 70 ºC with a 16:1 methanolsunflower oil molar ratio and different heterogeneous basic and acidic catalysts. The results showed that the microwave-heated reactions occur up to four times faster than those carried out with conventional heating. The reactions were performed with 24 catalysts; pure calcium oxide (CaO) and potassium carbonate, either pure or supported by alumina (K2CO3/Al2O3), were the most efficient catalysts.

MICROWAVE ACTIVATION OF IMMOBILIZED LIPASE FOR TRANSESTERIFICATION OF VEGETABLE OILS

This work investigated the effect of microwave irradiation (MW) on the ethanolysis rate of soybean and sunflower oils catalyzed by supported Novozyme 435 (Candida antarctica). The effects of tert-butanol, water addition and oil:ethanol molar ratio on transesterification were evaluated under conventional heating (CH), and under optimum reaction conditions (with no added water in the system, 10% tert-butanol and 3:1 ethanol-to-oil molar ratio). The reactions were monitored up to 24 h to determine the conditions of initial reaction velocity. The investigated variables under MW (50 W) were: reaction time (5.0-180 min) and mode of reactor operation (fixed power, dynamic and cycles) in the absence and presence of tert-butanol (10% (w/w). The measured response was the reaction conversion in ethyl esters, which was linked to the enzyme catalytic activity. The results indicated that the use of microwave improved the activity at fixed power mode. A positive effect of the association of tert-butanol and MW irradiation on the catalytic activity was observed. The reaction rate improved in the order of approximately 1.5 fold compared to that under CH with soybean oil. Using soybean oil, the enzymatic transesterification under MW for conversion to FAEE (fatty acid ethyl esters) reached >99% in 3h, while with the use of CH the conversions were about 57% under similar conditions.

Microwave Processes in Ferrite-ferroelectric Layered Structure

This work is devoted to investigation of wave processes in new hybrid ferrite/ferroelectric structures. Spin wave devices based on ferrite films have disadvanteges. And their applications are limited. Investigated structures allow to overcome disadvantages. This investigation helps to create new class of devices. Electromagnetic analysis of hybrid spin-electromagnetic waves in ferrite/ferroelectric structures were done. As a result dispersion relation was found. Numerical solution of this dispersion relation gave us follow results. These structures can be effectively tuned by external electric and magnetic field. Methods to increase tuning range were suggested. It was found that such structures have one basic disadvantage which is connected with presence of thick ferroelectric layer. To solve this problem is to use thin ferroelectric films. But this decreases tuning range. It was confirmed by experiment that this structures can be effectively tuned by electric and magnetic fields. Resonance characteristics of ferrite/ferroelectric resonator were succesfully tuned by magnetic and electric field.

Spectrophotometric determination of diclofenac in pharmaceutical preparations assisted by microwave oven

In this work, an effective and low-cost method for the determination of sodium or potassium diclofenac is proposed in its pure form and in their pharmaceutical preparations. The method is based on the reaction between diclofenac and tetrachloro-p-benzoquinone (p-chloranil), in methanol medium. This reaction was accelerated by irradiating of reactional mixture with microwave energy (1100 W) during 27 seconds, producing a charge transfer complex with a maximum absorption at 535 nm. The optimal reaction conditions values such as reagent concentration, heating time and stability of the reaction product were determined. Beer's law is obeyed in a concentration range from of 1.25x10-4 to 2.00x10-3 mol l-1 with a correlation coefficient of 0.9993 and molar absorptivity of 0.49 x10³ l mol-1 cm-1. The limit of detection (LOD) was 1.35x10-5 mol l-1 and the limit of quantification (LOQ) was 4.49x10-5 mol l-1. In the presence of the common excipients, such as glucose, lactose, talc, starch, magnesium stearate, sodium sulphite, titanium dioxide, polyethyleneglycol, polyvinylpirrolidone, mannitol and benzilic alcohol no interferences were observed. The analytical results obtained by applying the proposed method compare very favorably with those given by the United States Pharmacopeia standard procedure. Recoveries of diclofenac from various pharmaceutical preparations were within 95.9% to 103.3%, with standard deviations ranging from 0.2% to 1.8%.

Spectrometrical Monitoring of Laser Sintering Process of Ceramic Material

This thesis is done as a part of project called FuncMama that is a project between Technical Research Centre of Finland (VTT), Oulu University (OY), Lappeenranta University of Technology (LUT) and Finnish industrial partners. Main goal of the project is to manufacture electric and mechanical components from mixed materials using laser sintering. Aim of this study was to create laser sintered pieces from ceramic material and monitor the sintering event by using spectrometer. Spectrometer is a device which is capable to record intensity of different wavelengths in relation with time. In this study the monitoring of laser sintering was captured with the equipment which consists of Ocean Optics spectrometer, optical fiber and optical lens (detector head). Light from the sintering process hit first to the lens system which guides the light in to the optical fibre. Optical fibre transmits the light from the sintering process to the spectrometer where wavelengths intensity level information is detected. The optical lens of the spectrometer was rigidly set and did not move along with the laser beam. Data which was collected with spectrometer from the laser sintering process was converted with Excel spreadsheet program for result’s evaluation. Laser equipment used was IPG Photonics pulse fibre laser. Laser parameters were kept mainly constant during experimental part and only sintering speed was changed. That way it was possible to find differences in the monitoring results without fear of too many parameters mixing together and affecting to the conclusions. Parts which were sintered had one layer and size of 5 x 5 mm. Material was CT2000 – tape manufactured by Heraeus which was later on post processed to powder. Monitoring of different sintering speeds was tested by using CT2000 reference powder. Moreover tests how different materials effect to the process monitoring were done by adding foreign powder Du Pont 951 which had suffered in re-grinding and which was more reactive than CT2000. By adding foreign material it simulates situation where two materials are accidently mixed together and it was studied if that can be seen with the spectrometer. It was concluded in this study that with the spectrometer it is possible to detect changes between different laser sintering speeds. When the sintering speed is lowered the intensity level of light is higher from the process. This is a result of higher temperature at the sintering spot and that can be noticed with the spectrometer. That indicates it could be possible to use spectrometer as a tool for process observation and support the idea of having system that can help setting up the process parameter window. Also important conclusion was how well the adding of foreign material could be seen with the spectrometer. When second material was added a significant intensity level raise could be noticed in that part where foreign material was mixed. That indicates it is possible to see if there are any variations in the material or if there are more materials mixed together. Spectrometric monitoring of laser sintering could be useful tool for process window observation and temperature controlling of the sintering process. For example if the process window for specific material is experimentally determined to get wanted properties and satisfying sintering speed. It is possible if the data is constantly recorded that the results can show faults in the part texture between layers. Changes between the monitoring data and the experimentally determined values can then indicate changes in the material being generated by material faults or by wrong process parameters. The results of this study show that spectrometer could be one possible tool for monitoring. But to get in that point where this all can be made possible much more researching is needed.

Microwave-assisted solvent extraction and analysis of shikimic acid from plant tissues

A better method for determination of shikimate in plant tissues is needed to monitor exposure of plants to the herbicide glyphosate [N-(phosphonomethyl)glycine] and to screen the plant kingdom for high levels of this valuable phytochemical precursor to the pharmaceutical oseltamivir. A simple, rapid, and efficient method using microwave-assisted extraction (MWAE) with water as the extraction solvent was developed for the determination of shikimic acid in plant tissues. High performance liquid chromatography was used for the separation of shikimic acid, and chromatographic data were acquired using photodiode array detection. This MWAE technique was successful in recovering shikimic acid from a series of fortified plant tissues at more than 90% efficiency with an interference-free chromatogram. This allowed the use of lower amounts of reagents and organic solvents, reducing the use of toxic and/or hazardous chemicals, as compared to currently used methodologies. The method was used to determine the level of endogenous shikimic acid in several species of Brachiaria and sugarcane (Saccharum officinarum) and on B. decumbens and soybean (Glycine max) after treatment with glyphosate. The method was sensitive, rapid and reliable in all cases.

Optimized Fast-FISH with a-satellite probes: acceleration by microwave activation

It has been shown for several DNA probes that the recently introduced Fast-FISH (fluorescence in situ hybridization) technique is well suited for quantitative microscopy. For highly repetitive DNA probes the hybridization (renaturation) time and the number of subsequent washing steps were reduced considerably by omitting denaturing chemical agents (e.g., formamide). The appropriate hybridization temperature and time allow a clear discrimination between major and minor binding sites by quantitative fluorescence microscopy. The well-defined physical conditions for hybridization permit automatization of the procedure, e.g., by a programmable thermal cycler. Here, we present optimized conditions for a commercially available X-specific a-satellite probe. Highly fluorescent major binding sites were obtained for 74oC hybridization temperature and 60 min hybridization time. They were clearly discriminated from some low fluorescent minor binding sites on metaphase chromosomes as well as in interphase cell nuclei. On average, a total of 3.43 ± 1.59 binding sites were measured in metaphase spreads, and 2.69 ± 1.00 in interphase nuclei. Microwave activation for denaturation and hybridization was tested to accelerate the procedure. The slides with the target material and the hybridization buffer were placed in a standard microwave oven. After denaturation for 20 s at 900 W, hybridization was performed for 4 min at 90 W. The suitability of a microwave oven for Fast-FISH was confirmed by the application to a chromosome 1-specific a-satellite probe. In this case, denaturation was performed at 630 W for 60 s and hybridization at 90 W for 5 min. In all cases, the results were analyzed quantitatively and compared to the results obtained by Fast-FISH. The major binding sites were clearly discriminated by their brightness

STABILITY OF OILS HEATED BY MICROWAVE: UV - SPECTROPHOTOMETRIC EVALUATION

The effects of microwave heating on the oxidative stability of refined canola, corn and soybean oils were determined by absorptivity in the UV spectrum and by chemical analysis (peroxide and acid values). Samples were heated in a microwave oven (800 W, 2,450 MHz) for 0 to 36 min. Microwave heating produced oxidative degradation in the three oils. Absorptivity at 232 and 270 nm increased gradually with an increase in microwave exposure time (0-36 min) for canola, corn and soybean oils. Values of absorptivity at 232 nm increased from 4.812, 3.568 and 4.183 to 10.579, 12.874 and 15.950 after 36 min of heating canola, corn and soybean oil, respectively. The absorptivity at 232nm, due to the formation of conjugated dienes, was a good index for measuring the degradation of microwaved samples. UV scanning (220 - 320 nm) detected alterations in the spectrum of microwaved samples. Acid value also increased within 36 min of heating for all oils. Peroxide value showed a significant difference (P<0.05) in the initial stage of heating (0-6 min) for all oils. After this period it could not be correlated with absorptivity at 232 nm, due to the instability of hydroperoxides at high temperatures.

Physicochemical and sensory profile of rice bran roasted in microwave

The purpose of this study was to evaluate the physical, chemical, and sensory changes in bran from three rice cultivars according to microwave roasting time. This study analyzed three rice cultivars, BRS Sertaneja (S), BRS Primavera (P), and IRGA 417 (I) determining the color parameters (L*, a*, and b *) at 6, 9, 12, 15, and 18 minutes of roasting time. After applying the difference from control test, the rice brans with different characteristics aroma and flavor were selected: S and P roasted for 9 and 15 minutes and IRGA 417 roasted for 9, 12, and 15 minutes. These samples were characterized by Free-Choice Profile descriptive sensory analysis, and their chemical composition was also determined. The longer the roasting process, the higher the roasted flavor intensity and aroma. The IRG 417 cultivar roasted for 12 minutes showed a sweeter flavor and aroma. After roasting, the brans remained rich in protein and lipid and presented higher fiber content and lower reducing sugar and phytic acid content. Microwave roasting for 12 minutes can be a viable option for improving the sensory functional and nutritional characteristics of the rice bran considering its use in food products.

Convective, vacuum and microwave drying kinetics of mallow leaves and comparison of color and ascorbic acid values of three drying methods

Mallow leaves (Malva sylvestris L.) with initial moisture of 5.02±0.003 on dry basis (82.5% on wet basis) were dried using three different drying methods, microwave, convective and vacuum. The leaves that weigh 75 g each were dried until their moisture fell down to 0.10±0.005 on dry basis (approximately 9% on wet basis). The following drying levels were used in each of the drying processes: 6.67, 8.67, 10, 11.33 W g-1 microwave power density; 50, 75, 100 and 125 °C for convective drying; and 3, 7 kPa at 50 and 75 °C for vacuum drying. Drying periods ranged from 6-10, 26-150 and 38-130 min. for microwave, convective and vacuum drying, respectively. Effective moisture diffisuvities ranged from 2.04403 10-10-3.63996 10-12 m2 s-1, 1.70182 10-11-1.10084 10-10 m2 s-1 and 1.85599 10-11-5.94559 10-10 m2 s-1 for microwave, convective and vacuum drying, respectively. According to ascorbic acid content and color parameters, the best microwave power density was found 10 W g-1 with a drying period of 6.5 min.

Mathematical modeling of microwave dried celery leaves and determination of the effective moisture diffusivities and activation energy

Celery (Apium graveolens L. var. secalinum Alef) leaves with 50±0.07 g weight and 91.75±0.15% humidity (~11.21 db) were dried using 8 different microwave power densities ranging between 1.8-20 W g-1, until the humidity fell down to 8.95±0.23% (~0.1 db). Microwave drying processes were completed between 5.5 and 77 min depending on the microwave power densities. In this study, measured values were compared with predicted values obtained from twenty thin layer drying theoretical, semi-empirical and empirical equations with a new thin layer drying equation. Within applied microwave power density; models whose coefficient and correlation (R²) values are highest were chosen as the best models. Weibull distribution model gave the most suitable predictions at all power density. At increasing microwave power densities, the effective moisture diffusivity values ranged from 1.595 10-10 to 6.377 10-12 m2 s-1. The activation energy was calculated using an exponential expression based on Arrhenius equation. The linear relationship between the drying rate constant and effective moisture diffusivity gave the best fit.

Optimization of microwave drying conditions of two banana varieties using response surface methodology

AbstractOptimization of microwave drying conditions of Luvhele and Mabonde banana varieties were studied using response surface methodology. The drying was performed using a central composite rotatable design for two variables: microwave power level (100, 200 and 300 W) and drying time (40, 26, and 12 min.) for Luvhele; (100, 200 and 300 W) and (42, 27, and 12 min) for Mabonde. The colour and texture (hardness) data were analyzed using ANOVA and regression analysis. The fitness of the models obtained was good as the lack of fit for each of the models was not significant. The coefficient of determination R2 of the models was relatively high, hence the models obtained for the responses were adequate and acceptable. Drying conditions of 178.76 W, 12 min. drying time were found optimum for product quality at a desirability of 0.91 for Luvhele; while 127.67 W, 12 min. with a desirability of 0.86 was predicted for Mabonde. The result of this study could be used as a standard for microwave processing of Luvhele and Mabondebanana varieties.

Microwave-assisted extraction of anthocyanin from Chinese bayberry and its effects on anthocyanin stability

AbstractAnthocyanins are present in high concentrations in Chinese bayberry, Myrica rubra Sieb. & Zucc. Herein, a microwave-assisted extraction was used to extract the anthocyanins from Chinese bayberry. The HPLC chromatogram of the extracts showed that the anthocyanin components were slightly hydrolysed during the extraction process. Further experiments confirmed that microwave irradiation slightly hydrolysed cyanidin-3-O-glucoside to cyanidin, but did not significantly influence the antioxidant activity of the extracts. Optimized extraction conditions for total anthocyanin content were a solid-to-liquid ratio, extraction temperature, and extraction time of 1:50, 80 °C, and 15 min, respectively. Under these conditions, the anthocyanin content was 2.95 ± 0.08 mg·g−1, and the antioxidant activity yield was 279.96 ± 0.1 μmol.·g−1 Trolox equivalent on a dry weight basis. These results indicated that microwave-assisted extraction was a highly efficient extraction method with reduced processing time. However, under some extraction conditions it could damage the anthocyanins. These results provide an important guide for the application of microwave extraction.