Determinação da matéria-prima utilizada na produção do biodiesel adicionado ao diesel mineral através de monitoramento seletivo de íons

The selective ion monitoring acquisition mode in mass spectrometry was applied to identify, in the diesel complex matrix, the raw materials (vegetable oil and alcohol) that originate biodiesel. Biodiesel samples obtained from babassu, castor, palm and soybean vegetable oils and pure fatty acid methyl and ethyl esters were used to develop this method, using specific fragments in mass spectrometry and the "window system" in gas chromatography. The commercial Brazilian B2 samples were found to be produced with soybean oil, transesterified with methanol.

Determinação de paládio em amostras biológicas aplicando técnicas analíticas nucleares

This study presents Pd determinations in bovine tissue samples containing palladium prepared in the laboratory, and CCQM-P63 automotive catalyst materials of the Proficiency Test, using instrumental thermal and epithermal neutron activation analysis and energy dispersive X-ray fluorescence techniques. Solvent extraction and solid phase extraction procedures were also applied to separate Pd from interfering elements before the irradiation in the nuclear reactor. The results obtained by different techniques were compared against each other to examine sensitivity, precision and accuracy.

Determinação espectrofotométrica de citrato de sildenafil em formulações farmacêuticas

This paper describes a simple and rapid spectrophotometric method for quantitative determination of sildenafil citrate based on its reaction with p-chloranil accelerated by hydrogen peroxide, producing a stable purple compound (λmax= 535 nm). In the absence of peroxide this reaction is very slow. The experimental conditions were optimized by using response surface methodologies. Beer's law is obeyed in a concentration range of 8.52 x 10-5 - 1.70 x 10-3 mol L-1 (r = 0.999). The detection limit was 1.96 x 10-5 mol L-1. The method was successfully applied for the determination of sildenafil citrate in medicines with good accuracy and precision.

Determinação simultânea dos ácidos orgânicos tartárico, málico, ascórbico e cítrico em polpas de acerola, açaí e caju e avaliação da estabilidade em sucos de caju

The aim of the present study was determining the main organic acids in pulp and juices, as well as evaluating their stability, after opening the package, by liquid chromatography in a C18 column with isocratic elution and UV detection. In açaí pulp tartaric, malic and citric acids were found. Cashew samples presented all of the organic acids evaluated, besides high concentrations of ascorbic and malic acids. Acerola pulp had the highest ascorbic acid concentration. A small decrease in organic acid content during storage was observed. Malic and citric acids seem to be more stable than tartaric and ascorbic acids.

Aplicação de adsorção para remover amônia de efluentes suinícolas pré-tratados

The aim of this work is to evaluate the use of natural zeolites to remove the NH4+ that remains in effluents from swine facilities which were submitted to physico-chemical and biological treatments. Experiments were made in batch made adding 5% (w/w) of adsorbent (0.6-1.3 and 3.0-8.0 mm) to synthetic and real swine facilities effluents. The results show that ammonium removal is influenced by adsorbent particle size and the presence of other ions in the effluent. The adsorption equilibrium was described by Langmuir as well as Freundlich isotherms and the kinetic data fitted well a pseudo-second order model.

Validação de métodos cromatográficos para a determinação de resíduos de medicamentos veterinários em alimentos

Different agencies that supply validation guidelines worldwide establish almost the same parameters to be evaluated in the validation process of bioanalytical methods. However, they recommend different procedures, as well as establish different acceptance criteria. The present review delineates and discusses the stages involved in the validation procedures of bioanalytical methods designed for determining veterinary residues in food, explaining the main differences in the guidelines established for this purpose by the main regulatory agencies in the world.

Determinação espectroscópica multivariada de glucosamina e condroitina em formulações farmacêuticas

The objective of this study was to develop and validate an analytical method for quantification of glucosamine and chondroitin in pharmaceutical formulations. Multivariate calibration combined with infrared spectrophotometry allowed this analysis. 25 mixtures of glucosamine-6-sulphate and chondroitin-6-sulphate were used for calibration. Average errors found with this model during external validation were 1.37% for glucosamine sulphate and 1.30% for chondroitin sulphate. This method presented satisfactory results for assessed variables, what indicating that it is suitable for simultaneous quantification of glucosamine and chondroitin.

Determinação voltamétrica de metais em águas e fluidos biológicos empregando mineralização de amostras com radiação ultravioleta

This work describes the optimization of pretreatment steps for the destruction of organic matter in samples of waters and biological fluids, by using an UV irradiation system with a high power UV radiation source (400 W). The efficiency of the system constructed for the photo-decomposition of samples of model waters, natural waters and biological fluids was investigated by performing recovery experiments of the metallic species Zn(II), Cd(II), Pb(II), Cu(II), Al(III) and Fe(III). The use of UV irradiation allowed the liberation of metals bound to the organic matrix and the determination of the total content of elements in the samples.

Técnicas de extrações e procedimentos de clean-up para a determinação de hidrocarbonetos policílicos aromáticos (HPA) em sedimentos da costa do Ceará

Extraction and clean-up are essential points in polycyclic aromatic hydrocarbon (PAHs) analysis in a solid matrix. This work compares extraction techniques and clean-up procedures for PAH analysis. PAH levels, their toxicological significance and source were also evaluated in the waters of the Cocó and Ceará rivers. The efficiency of PAH recovery was higher for the soxhlet and ultrasonic techniques. PAH recovery varied from 69.3 to 99.3%. Total PAH concentration (ΣHPA) varied from 720.73 to 2234.76 µg kg-1 (Cocó river) and 96.4 to 1859.21 µg kg-1 (Ceará river). The main PAH sources are pyrolytic processes and the levels were classified as medium so that adverse effects are possible.

Otimização de método para determinação de flavonóis e flavonas em frutas por cromatografia líquida de alta eficiência utilizando delineamento estatístico e análise de superfície de resposta

This work optimized the HPLC conditions for the simultaneous determination of luteolin, apigenin, myricetin, quercetin and kaempferol in aglycone form, as well defined the best conditions for hydrolysis/extraction of these flavonoids in fruits, using the statistical central composite design and response surface analysis. A reverse phase method was developed using a gradient of methanol/water acidified with 0.3% formic acid as mobile phase and a photodiode array detector. The samples were extracted with methanol/water (50:50 v/v) at 90 ºC. The optimum time and HCl concentration varied for the different fruits investigated, demonstrating the necessity of optimizing these conditions for each fruit analyzed. Good recovery (87.1 to 96.3%), repeatability and linearity were obtained.

Determinação voltamétrica de ciclamato de sódio em produtos dietéticos empregando um eletrodo de diamante dopado com boro

The use of square-wave voltammetry in conjunction with a cathodically pre-treated diamond electrode for the analytical determination of sodium cyclamate is described. The samples were analyzed as received in a 0.5 mol L-1 H2SO4 solution in the concentration range from 5.0 × 10-5 mol L-1 to 4.1 × 10-4 mol L-1, with a detection limit of 4.8 × 10-6 mol L-1. The RSD was smaller than 1.2 % and the proposed method was applied with success in the determination of sodium cyclamate in several dietary products.

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.

Determinação quantitativa de TNT e HNS por TG e FT-IR

2,4,6-trinitrotoluene (TNT) is an energetic material that shows scarce crystalline properties that can be improved by addition of 2,2',4,4',6,6'-hexanitrostilbene (HNS) in the crystallization process. HNS is a very important high explosive used in a variety of military, aerospace and industrial formulations owing to its suitable properties. It is an insensitive and thermal stable explosive that can be produced from 2,4,6-trinitrotoluene (TNT). The purpose of this work is the quantitative determination of HNS and TNT in explosives by thermogravimetric analysis (TG) and Fourier transform infrared spectroscopy (FT-IR).

A espectrometria atômica e a determinação de elementos metálicos em material polimérico

Polymeric materials are widely used in the chemical industry and are part of our daily lives. Inorganic species may be added to them as additives, anti-oxidizing agents, stabilizers, plasticizers, colorants and catalysts and may be present in a wide range of concentrations. Their determination demands the development of analytical methods considering different kinds of polymeric materials, their composition and the final use of the material. Although many different analytical techniques may be used, this review emphasizes those based on atomic absorption and emission spectrometry. Solid sampling techniques and digestion methods are described and discussed and compared considering published results.

Uso de scanner em espectrofotometria de absorção molecular: aplicação em experimento didático enfocando a determinação de ácido ascórbico

Quantitative analysis of colored substances is generally performed using a spectrophotometer for detection of radiation. However, the combination of digital images and mathematical conversion of colors is an alternative for quantitative procedures based on colored chemical reactions. This work proposes a didactic experiment using a scanner for determination of ascorbic acid in medicines based on the formation of the Prussian blue complex. Results were in good agreement with a conventional spectrophotometer method and the procedure is attractive for instrumental analysis undergraduate courses.