Metodologias analíticas para determinação das fumonisinas em milho e alimentos à base de milho

Fumonisins are mycotoxins occurring worldwide, mainly in maize and maize-based food products, which could affect animal and human health. This paper reviews analytical methodologies for the determination of these fungal toxins in foods. It includes extraction, cleanup, derivatization procedures, detection, quantification, and confirmation procedures. Initial attempts at gas chromatographic methods and thin layer chromatography were supplanted by liquid chromatographic methods, mainly performed with fluorometric detection, or mass spectrometry detection, enabling the analysis of polar and thermolabile chemicals without chemical derivatization, which results in lower limits of detection. Alternative methods, such as enzyme linked immunosorbent assay or zone capillary zone electrophoresis, are also described.

Caracterização de 2,2',4,4',6,6'-hexanitroestilbeno via análises instrumentais

2,2',4,4',6,6'-hexanitrostilbene (HNS) is a very important high explosive that is used in a range of military, aerospace and industrial formulations owing to its suitable properties. It is an insensitive and thermaly stable explosive that can be produced from 2,4,6-trinitrotoluene (TNT). This paper shows the characterization of synthesized HNS by different techniques, such as elementary analysis, differential scanning calorimetry (DSC), thermogravimetric analysis (TG), Fourier transform infrared spectroscopy (FT-IR) and through the determination of the heat of combustion in a calorimeter.

Análises quali- e quantitativa de cafés comerciais via ressonância magnética nuclear

Coffee is one of the beverages most widely consumed in the world and the "cafezinho" is normally prepared from a blend of roasted powder of two species, Coffea arabica and Coffea canephora. Each one exhibits differences in their taste and in the chemical composition, especially in the caffeine percentage. There are several procedures proposed in the literature for caffeine determination in different samples like soft drinks, coffee, medicines, etc but most of them need a sample workup which involves at least one step of purification. This work describes the quantitative analysis of caffeine using ¹H NMR and the identification of the major components in commercial coffee samples using 1D and 2D NMR techniques without any sample pre-treatment.

Metodologia analítica para determinação de folatos e ácido fólico em alimentos

The aim of this work was to develop and to validate a methodology using HPLC for the simultaneous determination of folates and folic acid in foods. The limits of detection and the recovery rates for the vitamins in the certified reference materials were respectively 5 pg/mL and 94-108% for 5-MTHF, 7 pg/mL and 97-102% for THF, 30 pg/mL and 97.9-104% for 5-FTHF, 30 pg/mL and 95-107 for 10-FFA, 5 ng/mL and 97-102% for FA and 5 ng/mL and 98-103% for 10-MFA. Repeatability showed a coefficient of variation below 3.9% for all the vitamins. The proposed methodology was shown to be efficient when applied to different certified reference materials, namely pig's liver (BCR487), powdered milk (BCR421) and a vegetable mixture (BCR485).

Teores de corantes artificiais em alimentos determinados por cromatografia líquida de alta eficiência

Synthetic dyes are much used in processed foods. HPLC was applied to different types of snacks, such as colored cereals, chocolate confetti, chewing gums and candies for the determination of those additives. In the case of artificially colored breakfast cereals, 71% of the samples exceeded the allowed limits. Regarding the portions recommended for consumption by the makers of two of the samples, the amounts exceeded those allowed by the Brazilian legislation. In the case of chocolate confetti and candies none of the samples showed higher amounts than those allowed. However 37% of the chewing gum samples presented larger contents than the authorized ones, and one sample contained five times more synthetic dyes than allowed.

Surfactina: propriedades químicas, tecnológicas e funcionais para aplicações em alimentos

Surfactin, a lipopeptide produced by strains of Bacillus subtilis, has been proved to be a suitable biosurfactant in several applications. For many years, it has been investigated mainly for oil recovery and environmental usage. Its chemical, technological and functional characteristics turn surfactin into an attractive compound for several utilizations. In this review we emphasize some aspects of surfactin as a new food ingredient and its potential pharmaceutical and health applications.

Uso da pressão gerada por uma coluna de água para controle da vazão em sistemas de análises em fluxo

This work presents a new approach to control the flow rate in hydrodynamic flow experiments. The combination of air pressure generated by an aquarium air pump and the pressure generated by a water column were used for this purpose. This device supports a stable flow rate without pulsation for a long period of time. Furthermore, the flow rate can be easily controlled at various values in one or more streams. The performance of this approach was investigated using Fe(CN)6(4-) solutions in flowing systems using amperometric and voltammetric detection in wall-jet configuration. The results showed that the performance of the proposed device was better than a commercial peristaltic pump. It suggests that this approach can be used successfully in flow analysis systems.

O enfoque da metrologia química em análises toxicológicas na atividade turfística: validação de método analítico para determinação de cafeína em matrizes biológicas

This paper proposes an alternate method to detect forbidden doping substances present in biological matrices of horseracing. The method was fully validated for caffeine, identified as the most frequent forbidden substance in the analysis conducted by the Antidoping Laboratory of the Brazilian Jockey Club, which adopts a zero threshold limit according to national and international horseracing practices. The metrological reliability of the method applied to toxicological analysis in biological matrices is discussed. Although the analytical method proposed for detection of a zero threshold level of the doping substance is qualitative, it was validated for the determination of the limiting value (also known as quantification limit value) introducing a criterion that prevents the issuing of incorrect results ("false-positives" and "false-negatives").

Microssistemas de análises químicas: introdução, tecnologias de fabricação, instrumentação e aplicações

The amazing world of micro total analysis systems has provided a true revolution in analytical chemistry in recent years. The application of the microfluidic devices for chemical and biochemical processing has attracted considerable interest due to its advantages such as reduced sample and reagent consumption, processing time, energy, waste, cost, and portability. The aim of the present report is to disseminate the state of the art related to the miniaturization science in Analytical Chemistry. Historical progress, microfabrication technologies, required instrumentation and applications of the mTAS are presented in the current article, with special attention to the Brazilian contributions.

Modificação química e física do amido de quirera de arroz para aproveitamento na indústria de alimentos

The study evaluated the efficiency of chemical (phosphorylation) and physical (extrusion) modifications of the starch of broken rice. Results demonstrated a reduction in the moisture content of extruded and phosphorylated broken rice and an increase in the ash content of phosphorylated broken rice. Both phosphorylation and extrusion increased cold water binding capacity, swelling power, and solubility. Extruded and phosphorylated pastes were stable under refrigeration, but only extruded paste was stable when submitted to freezing. Phosphorylated paste had the lowest viscosity and the highest stability during heating, while the extruded one gelatinized without heating, but had higher losses during heating.

O estado da arte da cromatografia associada à espectrometria de massas acoplada à espectrometria de massas na análise de compostos tóxicos em alimentos

Chromatography combined with several different detection systems is one of the more used and better performing analytical tools. Chromatography with tandem mass spectrometric detection gives highly selective and sensitive analyses and permits obtaining structural information about the analites and about their molar masses. Due to these characteristics, this analytical technique is very efficient when used to detect substances at trace levels in complex matrices. In this paper we review instrumental and technical aspects of chromatography-tandem mass spectrometry and the state of the art of the technique as it is applied to analysis of toxic substances in food.

Estudo da mobilização de metais e elementos traços em ambientes aquáticos do semi-árido brasileiro aplicando análises de componentes principais

The spatial and temporal retention of metals has been studied in water and sediments of the Gavião River, Anagé and Tremedal Reservoirs, located in the semi-arid region, Bahia - Brazil, in order to identify trends in the fluxes of metals from the sediments to the water column. The determination of metals was made by ICP OES and ET AAS. The application of statistical methods showed that this aquatic system presents suitable conditions to move Cd2+ and Pb2+ from the water column to the sediment.

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.

Aplicação e avanços da espectroscopia de luminescência em análises farmacêuticas

This paper provides a review on the latest advances and applications of the luminescence spectroscopy for the development of pharmaceuticals analyses methods, basically based on the photo- and chemiluminescence. The different forms of the drugs determination on pharmaceuticals through the fluorescence and chemiluminescence are discussed. The analyses include the drugs native fluorescence (liquid and solid-phases); the fluorescence from the oxidizing or reducing forms of the drug; the fluorescence from the chemical derivatization and their photochemistry and hydrolysis reactions. The quenching of luminescence and chemiluminescence generation for the pharmaceutical quantification are also shown. Finally, the trends and future perspectives of the luminescence spectroscopy in the field of the pharmaceutical research are discussed.

Avaliação de uma proposta contextualizada sobre o ensino de polarimetria nos cursos de farmácia e engenharia de alimentos, na Universidade Federal do Ceará

This work deals with an evaluation of an experimental application about polarimetry for pharmacy and food engineering courses. Foods obtained from the undergraduate students were used for demonstrating multidisciplinary concepts and these concepts were associated to the teaching of polarimetry. According to the results, the benefits of the contextualization are beyond the class and the undergraduating students became interested in control of quality of foods. From these results, it can be concluded that the experimental emphasis given is valid and creates motivation and interest for learning physico-chemistry, in comparison with the traditional methodology applied to teach polarimetry.