Otimização de metodologia para derivação de desoxinivalenol através de planejamento experimental

The objective of this work was to optimize the derivatization reaction for determining deoxynivalenol (DON) by gas chromatography employing an experimental planning procedure. The factors were: temperature, reaction time, catalyst and trifluoroacetic anhydride concentration. The relative peak areas were used to evaluated the effects. The best conditions for DON derivatization were 200 µL TFAA and 18 mg sodium bicarbonate for 6 min at 74 ºC for 7 to 21 µg of DON. Under these conditions, the detection limit was 1.4 µg of DON.

Ciclização do lapachol induzida por sais de tálio III

This work describes the cyclization of lapachol (1) induced by thallium triacetate (TTA) and thallium trinitrate (TTN) in several solvents using magnetic stirring and under microwave irradiation. alpha-Xyloidone (2) - dehydro-alpha-lapachone - was obtained as the main product in these reactions in 20 75% yield. However, rhinacanthin-A (4) was isolated as main product in a 40% yield, using TTA and acetic anhydride:water (1:1) as solvent, and dehydro-iso-alpha-lapachone (3) in 21% yield, using TTA and dichloromethane as solvent. The reaction time decreased drastically under microwave conditions, but the yields of these reactions were not the expected.

Interesterificação química de óleo de soja e óleo de soja totalmente hidrogenado: influência do tempo de reação

Chemical interesterification is an important alternative to produce zero trans fats. In practice, however, excessive reaction times are used to ensure complete randomization. This work evaluated the influence of the reaction time on the interesterification of soybean oil/fully hydrogenated soybean oil blend, carried out in the following conditions: 100 ºC, 500 rpm stirring speed, 0.4% (w/w) sodium methoxide catalyst. The triacylglycerol composition, solid fat content and melting point analysis showed that the reaction was very fast, reaching the equilibrium within 5 min. This result suggests the interesterification can be performed in substantially lower times, with reduction in process costs.

Influência da ação das enzimas alcalase e flavourzyme no grau de hidrólise das proteínas de carne de frango

To study the action of Alcalase and Flavourzyme on the proteins of chicken meat, the influence of the substrate concentration [S], enzyme concentration [E] and hydrolysis time on the degree of hydrolysis (DH) of the proteins was evaluated. The highest DH for breast meat was obtained with a [S] of 3.3% (w/v), with a [E] of 6% (w/w) and reaction time of 90 min, for both enzymes. For thigh meat the conditions to get the highest DH were: [S] of 5% (w/v), [E] of 8% (w/w) and a reaction time of 120 min, for both enzymes.

Determination of Ni(II) in metal alloys by spectrophotometry UV-Vis using dopasemiquinone

A spectrophotometric method was proposed for Ni(II) determination in alloys using a dopa-semiquinone (L-1) to form [Ni(II)(L1-)3]1-, ε = 9.3 x 10³ L mol-1 cm-1. The optimal conditions for the determination were: wavelength 590 nm, temperature 25 °C, reaction time 45 min and pH 7.5. The Beer's law was obeyed for nickel from 3.33 x 10-5 to 1.78 x 10-4 mol L-1. The method was applied to complex samples, such as inox, nickel-titanium and cobalt-chromium alloys. A study of the potential interferents revealed that Mn was the major interferent. The limit of detection and quantification were 2.88 x 10-5 mol L-1 and 3.06 x 10-5 mol L-1, respectively.

Produção de biodiesel através de transesterificação in situ de sementes de girassol via catálise homogênea e heterogênea

The objective of this work is to show the results of the in situ transesterification of sunflower seed oil with methanol on basic homogeneous and heterogeneous catalysis for the production of biodiesel. In homogeneous catalysis, the activity of KOH and K2CO3 were evaluated using the same oil:methanol ratio of 1:90. KOH showed to be more active than K2CO3, leading to total conversion in biodiesel after 1h reaction time. In the heterogeneous catalysis the activity of K2CO3/Al2O3 was comparable to the activity of K2CO3 bulk: 53.0 and 66.6% resp. The properties of samples of biodiesel produced by homogeneous and heterogeneous catalysis were evaluated and are in accordance with the recommended fuel properties.

Síntese hidrotermal assistida por micro-ondas como metodologia sintética eficiente para obtenção da rede metalorgânica [ZN(BDC)(H2O)2]n

This work presents the optimization of the microwave-assisted hydrothermal synthesis of [Zn(BDC)(H2O)2]n . The reactions were carried out at the fixed temperature of 120 ºC for 10, 20, 30 and 40 min. Pure crystalline [Zn(BDC)(H2O)2]n was obtained in high yield (ca. 90%) with a reaction time of 10 min. The phase obtained and its purity was confirmed by Rietveld refinement, with a final value for Rwp/Rexp equal to 1.48. Increased reaction times (20, 30 and 40 min) favored the formation of unwanted by products, resulting in mixtures of several crystalline phases.

Spectrophotometric determination of famotidine using sulphonphthalein dyes

Four new extraction-free spectrophotometric methods have been established for the quantitation of famotidine (FMT). The methods are based on the formation of yellow ion-pair complexes between FMT and four sulphonphthalein dyes viz., bromothymol blue (method A), bromophenol blue (method B), bromocresol purple (method C) and bromocresol green (method D) in dioxane or acetone medium. The experimental variables such as reagent concentration, solvent medium and reaction time have been carefully optimized to achieve the highest sensitivity. The proposed methods were applied successfully to the determination of famotidine in tablets with good accuracy and precision and without interferences from common excipients. The results obtained by the proposed methods were compared favorably with those of the reference method.

Efficient synthesis of sulfonamide derivatives on solid supports catalyzed using solvent-free and microwave-assisted methods

In this work we report the synthesis of sulfonamide derivatives using a conventional procedure and with solid supports, such as silica gel, florisil, alumina, 4Å molecular sieves, montmorillonite KSF, and montmorillonite K10 using solvent-free and microwave-assisted methods. Our results show that solid supports have a catalytic activity in the formation of sulfonamide derivatives. We found that florisil, montmorillonite KSF, and K10 could be used as inexpensive alternative catalysts that are easily separated from the reaction media. Additionally, solvent-free and microwave-assisted methods were more efficient in reducing reaction time and in increasing yield.

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.

Iodeto de potássio suportado em peneiras moleculares mesoporosas (SBA-15 e MCM-41) como catalisador básico para síntese de biodiesel

Iodide potassium incorporated on mesoporous molecular sieves (SBA-15 and MCM-41) was used as heterogeneous catalysts in the transesterification of sunflower oil under different conditions of reaction time and ratio catalyst/oil (w/w). The results have showed that the system supported in SBA-15 has been more active than the supported in MCM-41, promoting a conversion to methyl esters of 84.98%.

Tratamento do efluente do biodiesel utilizando a eletrocoagulação/flotação: investigação dos parâmetros operacionais

Electrocoagulation/flotation process was applied to treat biodiesel wastewater using aluminium electrodes. Firstly, a literature survey was conducted to choose the process variables and then, operational parameters including initial pH, electrode distance and reaction time were tested. Experimental results showed the best parameter that can be used in a factorial design for further studies. The results indicate that electrocoagulation/flotation is very efficient to reduce oil and grease, the effluent was very clear after treatment and small amount of sludge was produced.

Epoxidação do óleo de soja com o sistema catalítico [MoO2(acac)2]/TBHP EM [bmim][PF6]

Epoxidation of soybean oil was investigated using 1-n-butyl-3-methylimidazolium hexafluorophosphate [bmim][PF6] ionic liquid as biphasic medium with molybdenum(VI) acetylacetonate complex and tert-butyl hydroperoxide TBHP as oxidizing agent. Reaction conditions were molar ratio TBHP:number of double bonds of oil:catalyst of 100:100:1, reaction temperature of 60 ºC and reaction time between 2 and 24 h. The proposed system showed catalytic activity for epoxidation reactions under tested conditions. Reuse of ionic liquid/catalyst system for epoxidation reactions was also investigated. Evaluation of epoxidation observed in this catalytic system was done by quantitative ¹H NMR data.

Otimização da esterificação de ácido hexanóico com n-butanol empregando lipase (Termomyces lanuginosus) imobilizada em gelatina

The application of Lipozyme (Termomyces lanuginosus) immobilized in gelatin gel in aliphatic ester synthesis was investigated taking the esterification of hexanoic acid with n-butanol as a model reaction. Conditions were optimized by factorial design and the highest conversion was obtained under the following conditions: molar ratio alcohol: acid of 2:1, reaction time of 48 h and biocatalyst weight of 7.0 g. Under these conditions the esterification yield was around 98 %. The operational stability of the immobilized lipase was assessed and results showed that after 12 batch runs, the enzyme showed no significant loss of activity.

A new approach to evaluate immobilization of β-galactosidase on Eupergit® C: structural, kinetic, and thermal characterization

This study aimed to evaluate β-galactosidase immobilization. For this purpose, the ionic strength of the buffer, reaction time, amount of the immobilization support, and pH were evaluated by a central composite design. Assay 8, which consisted of 1.5 mol L-1 phosphate buffer (pH 7.5) and a reaction time of 2 h, produced the maximum yield. Eupergit® C (400 mg) was subsequently used as an immobilization support. Immobilization kinetics wereinvestigated, and a significant increase in the yield was obtained after immobilization compared with that obtained from assay 8 (22.0 U mL-1 vs. 15.6 U mL-1). The enzyme efficiency of actuation was evaluated using o-nitrophenyl-β-D-galactopyranoside and lactose, with lactose providing better results. The reuse of β-galactosidase was evaluated, and more than 50% of the initial enzyme activity was maintained after five cycles of use. Enzyme characterization revealed that immobilization improved some aspects of the thermostability of β-galactosidase.