Desenvolvimento de metodologia analítica para determinação de colesterol em ração para ruminantes através de planejamento experimental fatorial

A chromatographic method was developed for cholesterol determination in feed for ruminants using response surface methodology. Among the five approaches of sample preparation methods tested, the saponification of the sample without heating presented less interference in the gas chromatography. The method presented a relative standard deviation (RSD) of 4.3%, recoveries between 84 and 87% and detection limit of 0.001 mg of cholesterol per g of feed.

Aplicação da metodologia de superfície de resposta no estudo da produção e extração da poligalacturonase

The aim of this work was to verify the effects of initial medium moisture content (U), addition of ammonium sulphate (N) and of potassium phosphate (P) in the production of the polygalacturonase through the solid-state fermentation, using cashew apple husk as substrate and Aspergillus niger CCT0916 as transformation agent. We also studied the best extraction conditions of the produced enzyme. The best condition of production was with U of 40%, 1% of N and 0% of P being reached an activity of the poligalacturonase of 10.1 U/g. The best extraction condition is an agitation system with a time of 100 min and a solvent-fermented medium volume ratio of 5 mL/g.

Validação de metodologia analítica por cromatografia líquida de alta eficiência para quantificação de bupivacaína (S75-R25) em nanoesferas de poli(lactídeo-co-glicolídeo)

Bupivacaine (S75-R25, NovaBupi®) is an amide type local anesthetic widely used. The present work consists of the development and validation of analytical methodology for evaluation of NovaBupi® content in the poly-lactide-co-glycolide nanospheres (PLGA-NS) by high performance liquid chromatography. The separation was made using the reversed-phase column LC-18, acetonitrile/phosphate buffer 85:15 v/v as mobile phase and detection at 220 nm. The results obtained show that the analytical methodology is accurate, reproducible, robust and linear over the concentration range 10-220.0 g/mL of NovaBupi®. The method was applied to determine the encapsulation efficiency and evaluate the release profile of NovaBupi®, showing good results.

Desenvolvimento e validação de metodologia analítica por CLAE-IR para determinação de artemisinina em Artemisia annua L

The aim of this work was to develop and validate an analytical methodology for determination of artemisinin used as antimalaric. The method was based on high performace liquid chromatography, using a CN column with mobile phase composed of methanol : H2O 50:50 (V/V). The results showed that the method presented linearity from 50 to 1500 µg/mL. It was considered selective, accurate, precise according to the specific resolution from ANVISA, the Brazilian regulatory agency.

Emprego de metodologia enzimática na obtenção de extratos protéicos de farinha de trigo

An enzymatic method was used for obtaining protein extracts from wheat flour using an alkaline protease. Some parameters were evaluated aiming the optimization of this method: temperature (40-50 ºC); time (2-5 h); physical treatment of the sample (no treatment, ultra-turrax/16,000 rpm/5 min and ultrasound/120 W/10 min); enzyme:substrate ratio (E:S) of 5:100 - 10:100 and concentration of wheat flour (1:3, 1:5 and 1:10 w/v). The results showed that the best condition for protein extraction was that using the sample concentration of 1:3 (w/v), ultra-turrax, E:S of 10:100, at 40 ºC, 2 h, having reached an extraction yield of 88.53%.

Metodologia AGOA: a modelagem de clusters de hidratação no complexo aziridina···ácido fluorídrico

We present a theoretical study of solvent effect on C2H5N···HF hydrogen-bonded complex through the application of the AGOA methodology. By using the TIP4P model to orientate the configuration of water molecules, the hydration clusters generated by AGOA were obtained through the analysis of the molecular electrostatic potential (MEP) of solute (C2H5N···HF). Thereby, it was calculated the hydration energies on positive and negative MEP fields, which are maxima (PEMmax) and minima (PEMmin) when represent the -CH2- methylene groups and hydrofluoric acid, respectively. By taking into account the higher and lower hydration energy values of -370.6 kJ mol-1 and -74.3 kJ mol-1 for PEMmax and PEMmin of the C2H5N···HF, our analysis shows that these results corroborate the open ring reaction of aziridine, in which the preferential attack of water molecules occurs at the methylene groups of this heterocyclic.

Validação de metodologia para a determinação simultânea dos antioxidantes sintéticos em óleos vegetais, margarinas e gorduras hidrogenadas por CLAE/UV

The use of antioxidants either to prevent or retard food's lipids oxidation was approved after inquires that verified their security within a daily intake limit. In this study, the methodology was developed and validated for the analysis of synthetic antioxidants: propylgallate (PG), tert-butylhydroquinone (TBHQ), butylhydroxyanisole (BHA), octylgallate (OG) and butylhydroxytoluene (BHT) in vegetables oils, margarine and hydrogenated fats by high performance liquid chromatographic. The methodology revealed itself efficient, with recovery rates above 90% for all antioxidant substances, besides good linearity in concentration range of 40-240 mg kg-1 (r = 0,999), repeatability with CV < 3,7% and limit of quantification 16.55, 10.32, 1.40, 3.76 and 9.30 mg/kg for BHT, BHA, PG, OG and TBHQ, respectively.

Validação de metodologia para a caracterização química de bagaço de cana-de-açúcar

In this work, a methodology for the characterization of sugar cane bagasse was validated. Bagasse pre-treated with steam in a 5000 L reactor at a pressure of 15.3 kgf/cm², during 7 min, was used to test the methodology. The methodology consisted of the hydrolysis of the material with H2SO4 at 72% v/v, for the quantification of carbohydrates, organic acid, furfural and hydroxymethylfurfural by HPLC; insoluble lignin and ash by gravimetry; and soluble lignin by spectrophotometry. Linearity, repeatability, reproducibility and accuracy of the results obtained in two Research Laboratories were determined, and were considered to be suitable for the validation of the methodology.

Validação da metodologia da avaliação de incerteza em curvas de calibração melhor ajustadas por polinômios de segundo grau

The most widespread literature for the evaluation of uncertainty - GUM and Eurachem - does not describe explicitly how to deal with uncertainty of the concentration coming from non-linear calibration curves. This work had the objective of describing and validating a methodology, as recommended by the recent GUM Supplement approach, to evaluate the uncertainty through polynomial models of the second order. In the uncertainty determination of the concentration of benzatone (C) by chromatography, it is observed that the uncertainty of measurement between the methodology proposed and Monte Carlo Simulation, does not diverge by more than 0.0005 unit, thus validating the model proposed for one significant digit.

Otimização de metodologia analítica para o doseamento de flavonoides de Bauhinia cheilantha (Bongard) Steudel

The present study examined the optimization of stabilization and extraction processes of the flavonoids of Bauhinia cheilantha (Bongard) Steudel. Four drying temperatures (room temperature, 40, 60 and 80 ºC) and seven extraction systems (distilled water, 100% methanol, 80% methanol, 100% ethanol, 80% ethanol, 80% acetone and 60% acetone) were examined. The results demonstrated a reduction in flavonoid levels with increasing drying temperatures; and 80% acetone, 80% ethanol, and methanol p.a extraction systems were found to be most efficient and its weren't differents statisticaly (p<0.05).

Salinidade em petróleo bruto: otimização de metodologia e proposta de um novo método para extração de sais em petróleo

The quantity of salts in the crude oils depends on the origin and of the wells production and these salts cause several problems during the transport and the process of refine as corrosions, incrustations and deactivation of the employed catalysts in the refineries. In this study were implemented changes for improvements in the execution of ASTM D 6470 method and has also developed a new methodology of extraction system of salts using process of mechanical agitation without heating. The results of the optimization produce larger efficiency and safety to the process compared to the traditional ASTM method.

Validação de metodologia analítica para determinação de mercúrio total em amostras de urina por espectrometria de absorção atômica com geração de vapor frio (CV-AAS): estudo de caso

Mercury is a toxic metal used in a variety of substances over the course history. One of its more dubious uses is in dental amalgam restorations. It is possible to measure very small concentrations of this metal in the urine of exposed subjects by the cold vapor atomic absorption technique. The present work features the validation as an essential tool to confirm the suitability of the analytical method chosen to accomplish such determination. An initial analysis will be carried out in order to evaluate the environmental and occupational levels of exposure to mercury in 39 members of the auxiliary dental staff at public consulting rooms in the city of Araguaína (TO).

Desenvolvimento de metodologia para determinação de piretroides em manteiga

The objective of this study was to evaluate the use of the matrix solid-phase dispersion technique associated with purification at low temperature for the determination of pyrethroids in butter. Evaluated parameters included: sample/adsorbent ratio, type of adsorbent and extractor solvent. The optimized method was validated based on predetermined requirements. The detection limits of the pyrethroids cypermethrin and deltamethrin were 0.082 and 0.11 μg g-1, and quantification limit were 0.28 and 0.32 μg g-1, respectively, with extraction percentages near 90% and coefficients of variation less than of 10%..

Metodologia para o estudo da porosidade de dolomita em ensaio de sulfatação interrompida

The aim of this work is to propose a methodology to evaluate the evolution of the pore blockage of limestone during the sulfation reaction. The experiments were performed for a national limestone (dolomite) with average particle size of 545 μm in interrupted sulfation tests were conducted at seven different times and at three different temperatures of the process. The empirical data were obtained from porosimetry tests to establish BET surface area, volume and average size of pore and distribution of pore sizes of the sulfated samples. Thermogravimetric tests were performed to evaluate the preparation methodology of the samples used in the porosimetry tests.

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.