Validação de método analítico para determinar a migração de ε-caprolactama das embalagens para alimentos gordurosos

ε-Caprolactam (CAP) is a monomer of nylon 6 used as food packaging for bologna sausage, turkey blanquettes, fowl breast, pâtés and ham luncheon meat. After polymerization a part of the monomer can remain in the packaging and migrate into the food. The aim of this work was develop and validate a single laboratory method to determine CAP in ethanol 95% that simulates fatty food characteristics. Thus, linear range was 2 to 32 mg/L of CAP, detection and quantification limits were 0.83 and 1.63 mg/L, respectively. Repeatability showed Hor Rat values lower than 2 while recovery range was 97.5 to 106.5%. The method was considered adequate for purpose.

Uso da cromatografia gasosa bidimensional abrangente (GC×GC) na caracterização de misturas biodiesel/diesel: aplicação ao biodiesel de sebo bovino

The growth of biodiesel market and the implementation of regulations related to biodiesel production and biodiesel/diesel blending has encouraged the development of appropriate analytical methods to control the composition of this type of mixture. In this study, an evaluation of the potential of GC×GC for the characterization of samples of beef tallow biodiesel and the composition of blends of biodiesel/diesel is presented. The methodology was applied to beef tallow biodiesel and its mixtures with petrodiesel, ranging from B2 to B50. Results allowed not only the identification and quantification of the biodiesel esters, but also the biodiesel percentage in biodiesel/diesel blends.

Validação de método multirresíduo para determinação de pesticidas em alimentos empregando QuEChERS E UPLC-MS/MS

This paper presents a practical and rapid method which was validated for simultaneous quantification and confirmation of 29 pesticides in fruits and vegetables using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were extracted following the method known as QuEChERS. Using the developed chromatographic conditions, the pesticides can be separated in less than 9 min. Two multiple reaction monitoring (MRM) assays were used for each pesticide. Four representative matrices (lettuce, tomato, apple and grapes) were selected to investigate the effect in recoveries and precision. Typical recoveries ranged from 70-120%, with relative standard deviation (RSDs) lower than 20%.

Aspectos analíticos da resposta do detector de ionização em chama para ésteres de ácidos graxos em biodiesel e alimentos

The analysis of fatty acid (FA) esters by gas chromatography and flame ionization detector (FID) normally uses the normalization method. However, if one FA is wrongly estimated, the results could be greatly affected. In this study, methodologies using internal standards and correction factors for the FID response are described. The results show that by using theoretical correction factors associated to the internal standardization, the quantitative analyses of the FAs are expressed in mass, increasing the accuracy and facilitating the interpretation and comparison of the results for foods and biodiesels.

Caracterização de resíduo sólido formado em biodiesel de sebo bovino

The nature of the solid residue formed in beef tallow biodiesel from two commercial producers in Brazil was determined by comparative analytical techniques, namely, gas chromatography with flame ionization detector (GC-FID) and thermogravimetry (TG). Pure monopalmitin and monostearin were used as reference standards for both methodologies. Analyses were carried out before and after filtration of the solids formed, which allowed the observation that the formation of precipitate reduced the levels of monoglycerides in the beef tallow biodiesel. The chromatographic and thermogravimetric results confirmed the nature of the residue as saturated monoglycerides, predominantly monostearin and monopalmitin.

Aspectos analíticos e regulatórios na determinação de resíduos de macrolídeos em alimentos de origem animal por cromatografia líquida associada à espectrometria de massas

This is an overview of LC-MS techniques applied for macrolide determination in food, including sample preparation and method validation, as well as the policies adopted by international agencies regarding their presence in food. Techniques for the analysis of macrolides in food normally include solid phase or liquid-liquid extraction followed by HPLC. UHPLC presents advantages in running time, detectability and solvent consumption. Triple-quadrupoles are the most common analyzers in instruments used for the determination of contaminants in food, but time-of-flight and ion-trap spectrometers have been successfully applied for analyses focusing on the investigation of structural formula or the presence of degradation products.

O estado da arte na determinação de resíduos de medicamentos veterinários em alimentos de origem animal empregando técnicas cromatográficas acopladas à espectrometria de massas

The determination of veterinary drug residues in foods of animal origin is an important issue because of the risk these compounds pose to human health in addition to their persistence and tendency to bioaccumulate. In recent years, significant progress has been made in the area and this review presents the state of the art in sample preparation procedures associated with chromatographic techniques coupled to mass spectrometry for multiresidue determination of veterinary drugs in food of animal origin at concentration levels suitable for the control of residues and contaminants in food.

Chumbo e cádmio detectados em alimentos vegetais e gramíneas no município de Santo Amaro-Bahia

This study evaluated the level of the metals Pb mg kg-1 and Cd mg kg-1 found in plant species and the contribution of the levels detected in contaminated soils located in the urban area of the city of Santo Amaro, Bahia. Levels were determined by graphite furnace and flame atomic absorption spectrometry. The results showed the presence of Pb and Cd in plant species at levels ranging from 0.18 to 118.2 mg kg-1 and 0.04 to 7.29 mg kg-1, respectively. The concentration values obtained varied according to the plant species and were not strongly influenced by the concentration values detected in the soil.

Ésteres de cloropropanóis e de glicidol em alimentos

Chloropropanols are a well-known group of food processing contaminants. They are formed through the reaction between lipids and chlorides when submitted to thermal treatment, and can be found in free and bound form. Although free chloropropanols were identified around 30 years ago, the occurrence of bound forms, especially 3-MCPD, and glycidyl fatty acid esters, has only recently been reported in several food products. Dietary exposure to these ester-bound compounds has been considered a priority food safety issue since free forms can be potentially released through the action of gut lipases, representing a major toxicological concern.

Determinação de resíduos de agrotóxicos em leite bovino empregando método QuEChERS modificado e GC-MS/MS

Considering the possibility that pesticides used in cattle raising produce residues in milk and cause harm to public health, this study developed a multiresidue method for determination of pesticide residues in bovine milk, using a modified QuEChERS method for sample preparation, and quantification by GC-MS/MS. The method proved to be efficient, resulting in satisfactory recoveries in the range 71.1 to 117.4%, for 45 of the 48 compounds analyzed with RSD values < 17.3%. The method LOD and LOQ were3.0 and 10.0 µg L-1, respectively, except for cyfluthrin which showed 7.5 and 25.0 µg L-1.

Interação de complexo de rutênio com albumina de soro bovino para detecção amperométrica de ácido ascórbico

The binding of [Ru(PAN)(PPh3)2(ISN)]Cl (PAN = 1-(2'-Pyridylazo)-2-naphtholate) to bovine serum albumin (BSA) was investigated by spectroscopic techniques. According to analysis of the results from the Stern-Volmer equation, the ruthenium complex is able to quench the fluorescence intensity of BSA via a dynamic mechanism. The thermodynamic parameters were calculated (ΔH = 30.3 kJ mol-1; ΔS = 195.4 J mol-1 K-1), indicating that hydrophobic force is the main interaction driving force. The site marker competitive experiments revealed that the binding site of ruthenium complex was in the sub-domain IIA of BSA. FTO glass with a film of BSA-[Ru(PAN)(PPh3)2(ISN)]Cl was used as an ascorbic acid sensor. The linear range of the modified electrode was between 1 and 8 × 10-6 mol L-1.

MICROEMULSÕES: COMPONENTES, CARACTERÍSTICAS, POTENCIALIDADES EM QUÍMICA DE ALIMENTOS E OUTRAS APLICAÇÕES

Microemulsions (MEs) are thermodynamically stable systems consisting of nanosized droplets dispersed in a solvent continuous medium (known as pseudo-phase), which is immiscible with the dispersed phase. These systems consist of water, a hydrophobic solvent called "oil," an amphiphile and often, a co-surfactant that is normally a medium chain alcohol. A large number of publications describe the importance of MEs in many branches of chemistry, and there is an intensive search for new applications. In addition, MEs have been applied in many areas, including oil extraction, removal of environmental pollutants from soils and effluents, dissolution of additives in lubricants and cutting oils, cleaning processes, dyeing and textile finishing, as nanoreactors to obtain nanoparticles of metals, semiconductors, superconductors, magnetic and photographic materials, and latex. However, only some studies indicate the potential applications of MEs in food and even fewer evaluate their chemical behavior. Potential applications of MEs in food comprise dissolution of lipophilic additives, stabilization of nutrients and biologically active compounds, using as an antimicrobial agent and to maximize the efficiency of food preservatives. This work consists of a literature review focusing on composition and physical and chemical characteristics of microemulsions. Despite the small number of studies on the subject reported in the literature, we demonstrate some potential applications of MEs in food chemistry.

Emergência de plântulas de Zizyphus joazeiro Mart (Rhamnaceae) em função de substratos

O juazeiro é uma planta muito importante para a região semiárida do Nordeste, mantendo-se sempre verde e constituindo fonte de alimentos para os animais na época de escassez de chuvas. Devido ao fato de a espécie se propagar principalmente por unidades de dispersão (endocarpo + semente), este estudo teve como finalidade avaliar diferentes tipos de substratos para emergência de plântulas de juazeiro. O experimento foi conduzido em casa de vegetação, no Centro de Ciências Agrárias da Universidade Federal da Paraíba, em Areia, PB. Os substratos utilizados foram: Plugmix®, vermiculita, terra vegetal, terra vegetal + esterco bovino (nas proporções de 3:1, 1:1 e 1:3), terra vegetal + areia (nas proporções de 3:1, 1:1 e 1:3), areia, areia + pó de madeira (nas proporções de 3:1, 1:1 e 1:3), pó de madeira, areia + raspa de madeira (nas proporções de 3:1, 1:1 e 1:3), raspa de madeira, areia + esterco bovino (nas proporções de 3:1, 1:1 e 1:3). Através de avaliações diárias, determinaram-se as seguintes características: emergência, índice de velocidade de emergência, comprimento e massa seca de plântulas. Para emergência de plântulas, o substrato mais eficiente foi terra vegetal, e, quanto ao vigor, os maiores valores foram obtidos nos substratos Plugmix®, terra vegetal + esterco bovino, nas proporções de 3:1 e 1:1 e areia.

Variabilidad espacial de atributos físicos de un Typic Haplustox de los Llanos Orientales de Colômbia

O objetivo deste trabalho foi estudar o comportamento da variabilidade espacial da resistência mecânica à penetração (RP), da densidade do solo, da densidade de partículas do solo, da porosidade total e dos teores de areia, silte e argila, e as relações existentes entre as propriedades analisadas. O estudo foi desenvolvido em Puerto López (Meta-Colômbia). As amostras do solo foram coletadas em duas profundidades (0 - 0,10 e 0,10 - 0,20 m), em intervalos regulares de 25 m, em malha regular, compreendendo 42 pontos, sendo a RP medida até 0,42 m de profundidade. A RP não se correlacionou com nenhuma propriedade, na primeira profundidade. De 0,10 - 0,20 m de profundidade, a RP correlacionou-se com os teores de silte e areia. Os semivariogramas da RP não apresentaram correlação espacial nas duas profundidades, possivelmente devido ao sistema de preparo do solo, que modifica a dependência espacial na superfície, acarretando maior homogeneidade do solo. As propriedades ajustaram-se a modelos de semivariogramas exponenciais e esféricos. Para a profundidade de 0,10 - 0,20 m, as propriedades não se ajustaram a modelos de semivariogramas, apresentando efeito pepita puro, ou seja, não apresentaram dependência espacial, à exceção da densidade aparente.

Nova metodologia para interpretação de dados de análise sensorial de alimentos

Os métodos atualmente utilizados para realização de análise sensorial têm deixado muito a desejar por não traduzir satisfatoriamente os resultados. Diante deste problema, analisou-se a possibilidade de introdução de um fator que medisse o índice de concordância dos provadores sobre determinado aspecto analisado. Para validação deste coeficiente, foi avaliada a concordância entre julgadores na análise sensorial para três diferentes amostras de suco de pinha (Annona squamosa L.): uma constituída apenas do suco de pinha sem leite e duas com diferentes concentrações pinha/leite. Utilizou-se a Análise de Componentes Principais (ACP) e também a nova metodologia proposta pelos autores, com base na definição do desvio-padrão, aplicada às frequências absolutas das notas dos julgadores, para cada propriedade sensorial estudada. Com esta metodologia, definiu-se uma relação para o cálculo de uma medida de concordância entre os julgadores, denominada de coeficiente de concordância, a qual pode assumir valores de 0 a 100% e também permite comparações que não são possíveis, utilizando-se da ACP. Por fim, concluiu-se que tal metodologia é mais indicada que a ACP, na avaliação da concordância entre os julgadores na análise sensorial.