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%.

THE SKEPTICAL CARTESIAN BACKGROUND OF HUME'S "OF THE ACADEMICAL OR SCEPTICAL PHILOSOPHY" (FIRST INQUIRY, SECTION 12)

ABSTRACT In section XII of the First Inquiry, Hume refers to the two Hellenistic schools of skepticism (Academic and Pyrrhonian) to present his own view of skepticism, which, however, depends on the ancient skeptics mainly indirectly. Hume's view of skepticism depends crucially on Descartes and post-Cartesian philosophers such as Pascal, Huet, Foucher and Bayle, who reacted skeptically to major Cartesian doctrines but followed one version or other of Descartes's methodical doubt. Although all these post-Cartesian philosophers are relevant in section XII, I focus on the topics in which Descartes himself-besides his skeptical followers-seems directly relevant. After an introductory section (I) on Julia Annas' and Richard Popkin's views of Hume's relation to, respectively, ancient and modern skepticism, I turn to section XII and examine what Hume calls (II) "consequent skepticism about the senses," (III) "antecedent skepticism," and (IV) "Academic skepticism."

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

Effect of scanner acoustic background noise on strict resting-state fMRI

Functional MRI (fMRI) resting-state experiments are aimed at identifying brain networks that support basal brain function. Although most investigators consider a ‘resting-state’ fMRI experiment with no specific external stimulation, subjects are unavoidably under heavy acoustic noise produced by the equipment. In the present study, we evaluated the influence of auditory input on the resting-state networks (RSNs). Twenty-two healthy subjects were scanned using two similar echo-planar imaging sequences in the same 3T MRI scanner: a default pulse sequence and a reduced “silent” pulse sequence. Experimental sessions consisted of two consecutive 7-min runs with noise conditions (default or silent) counterbalanced across subjects. A self-organizing group independent component analysis was applied to fMRI data in order to recognize the RSNs. The insula, left middle frontal gyrus and right precentral and left inferior parietal lobules showed significant differences in the voxel-wise comparison between RSNs depending on noise condition. In the presence of low-level noise, these areas Granger-cause oscillations in RSNs with cognitive implications (dorsal attention and entorhinal), while during high noise acquisition, these connectivities are reduced or inverted. Applying low noise MR acquisitions in research may allow the detection of subtle differences of the RSNs, with implications in experimental planning for resting-state studies, data analysis, and ergonomic factors.

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.