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.

Processo de estabilização de resíduos orgânicos: vermicompostagem versus compostagem

Two processes are used to stabilize organic wastes: composting and vermicomposting.There are no studies in the literature showing which process is most effective over the short term. In this study, 3 organic wastes were composted and vermicomposted for 90 days, and the parameters pH, effective cation exchange capacity, total organic carbon, total Kjeldahl nitrogen, Ptotal, E4/E6 ratio, hydrophobicity and aromaticity indexes were determined. In all experiments, vermicomposted materials showed higher stability, proving a superior tool for stabilization of these organic wastes.

Compósitos biodegradáveis de amido de mandioca e resíduos da agroindústria

The objectives of this work were to produce biodegradable composites using starch and different agro-industrial wastes (coconut fiber, soy bran and sugarcane bagasse) using a baking process, and to study the effects of these components on the resultant composite properties. The addition of different residues yielded trays with different properties. Samples manufactured with soy bran showed the highest density and water uptake at relative humidities ≥ 60%. The addition of sugarcane bagasse resulted in less dense and resistant samples whereas coconut fiber composites showed the highest breaking stress. The samples fabricated in this study represent an alternative packaging option for foods with low water content.

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.

Resíduos de medicamentos veterinários em leite e ovos

The use of veterinary drugs in food producing animals may result in the presence of residues in foods, including milk and eggs. Immunoassay or microbiological tests are used to screen for residues, but chromatographic methods are needed to confirm positive results. In most methods, the sample is extracted with acetonitrile, submitted to clean up or directly analyzed by LC-MS/MS. Results of the Brazilian governmental monitoring programs from 2006 to 2011 have shown that the antiparasitic ivermectin was the drug most frequently found in milk. Residues in eggs are only monitored by one of the programs, and few studies have reported the incidence of veterinary drugs in this matrix in Brazil.

Obtenção e caracterização de matriz apropriada para sistemas de liberação prolongada: estudos de liberação dos herbicidas atrazina e diuron

This study aimed to produce and characterize a novel material from fish scales and chitosan for use as a medium for the extended release of herbicides. The mechanism of release for the herbicides atrazine and diuron was influenced by diffusion and swelling according to the power law kinetic model. The atrazine release time was seven days, while that of diuron was four days. The results of this study will contribute to the development of environmental matrices for herbicide release systems.

Caracterização físico-química de resíduos oleosos do saneamento e dos óleos e graxas extraídos visando a conversão em biocombustíveis

Oily waste from sanitation processes was characterized for its potential use in the generation of biofuels. The waste residues studied showed high levels of oil and grease, reaching up to 87% (m/m) in a grease trap of a food company, showing that these residues can be utilized for the production of biofuels. The results revealed high levels of moisture and saponification as well as high levels of free fatty acids (FFA). Analysis of chromatographic profiles (HPLC) showed great heterogeneity of the fatty acids contained in the sample, and a predominance of palmitic, oleic, linoleic and linolenic acids.

Produção de hidrogênio via fermentação anaeróbia - aspectos gerais e possibilidade de utilização de resíduos agroindustriais brasileiros

Biological production of hydrogen through anaerobic fermentation has received increasing attention and offers a great potential as an alternative process for clean fuel production in the future. Considering biological systems for H2 production, anaerobic fermentation stands out, primarily due to its higher production of H2 compared with other biological processes. In addition the possibility of using different agro-industrial wastes as substrates opens up infinite possibilities. The development and implementation of sustainable processes for converting renewable materials into different value-added products is essential for the full exploitation of Brazilian agro-industrial wastes.

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.

MONITORAMENTO DE RESÍDUOS DE AGROTÓXICOS DA CLASSE DOS ORGANOFOSFORADOS POR CGDFC EM AMOSTRAS DE LEITE FLUÍDO E EM PÓ

Samples of whole fluid pasteurized, UHT and powdered milk were analyzed for the presence of organophosphorus pesticide residues (OPR) using the QuEChERS method with detection by GC-FPD and confirmation by UPLC-MS/MS. A total of 23% of fluid milk samples and 27% of powdered milk samples contained at least one organophosphorus residue. The OPR found in the samples showed these can reach the milk and remain even after pasteurization, sterilization and drying processes. Some domestic sanitary residues were also present in the powdered milk samples. These residues have no LMR in Brazilian food legislation and are therefore not taken into account in food intake evaluations. There was an unidentified chromatographic peak in 30% of all the liquid and powdered milk samples, indicating the presence of some other contaminant.

PREPARAÇÃO E CARACTERIZAÇÃO DE MEMBRANAS DE CELULOSE REGENERADA A PARTIR DA CELULOSE EXTRAÍDA DE RESÍDUOS AGROINDUSTRIAIS PARA APLICAÇÃO EM PROCESSOS DE SEPARAÇÃO

The aim of this study was to produce membranes using the adapted cuprammonium method. The cellulose utilized was obtained from recycled agroindustrial residues: sugarcane bagasse, corn stover and soybean hulls. The levels of Cu (II) ions in regenerated cellulose membranes produced with cellulose from bagasse, corn stover and soybean hulls were 0.0236 wt%, 0.0255 wt% and 0.0268 wt%, respectively. These levels were approximately 15 times lower than those observed in previous studies (0.3634 wt%). Cellular viability data show that membranes produced from bagasse cellulose do not present toxicity to the cellular cultures studied. These results demonstrate an evolution in production of regenerated cellulose membranes from agroindustrial residues mainly due to a decrease in the Cu (II) ions level, showing the possibility of application of these systems with improved membranes processing.

Estudos sobre aplicações conjuntas de herbicidas e nematicidas sistêmicos na eficácia dos nematicidas em cana-de-açúcar

Com o objetivo de avaliar uma possível influência da aplicação conjunta de nematicidas sistêmicos e herbicidas sobre a eficácia dos nematicidas, no controle de Meloidogyne spp. e Pratylenchus zeae em cana-de-açúcar (híbrido de Saccharum spp.) no Nordeste, instalaram-se dois experimentos, um irrigado e outro não irrigado, ambos em canaviais nordestinos, há muito cultivados e comprovadamente infestados por fitonematóides. A variedade utilizada foi SP79-1011, os nematicidas aldicarb e terbufós e os herbicidas diuron, ametrina, oxyfluorfen e pendimetalin, aplicados no plantio, nas doses recomendadas comercialmente. As avaliações fundamentaram-se nos níveis populacionais dos nematóides observados em três diferentes momentos, e nos fatores de reprodução. Avaliaram-se também o desenvolvimento das plantas, a produtividade agrícola e dois parâmetros tecnológicos. Os resultados demonstraram que não houve efeito dos herbicidas na eficácia dos nematicidas, nem foram significativas as diferenças em relação à produtividade, exceto na área irrigada, para perfilhamento nos tratamentos com herbicidas, e número de colmos e perfilhos, nos tratamentos com nematicidas em relação à testemunha. Os nematicidas e herbicidas não afetaram os níveis de Pol e PCC do caldo, não interferindo, portanto, na produtividade industrial. Houve interação estatística entre nematicida e herbicida para P. zeae na rizosfera, na área irrigada, com a menor população do parasito encontrada na combinação aldicarb + pendimetalin.

Determinação de ácidos carboxílicos em composto de resíduos sólidos urbanos por cromatografia gasosa com detector de ionização em chama

Um método simples e eficiente para determinação simultânea de quatro ácidos carboxílicos de cadeia curta (acético, propiônico, butírico e valérico) em resíduos sólidos urbanos (RSU) é descrito no presente trabalho. Estes ácidos são considerados fitotóxicos na literatura e a variabilidade das suas concentrações durante o processo pode ser usada como parâmetro da maturação do composto de resíduos sólidos urbanos (RSU). A determinação dos ácidos carboxílicos presentes no composto de RSU envolve uma extração em água e filtração em membranas de polifluoreto de vinilideno (PVDF), seguida da injeção direta em um cromatográfo a gás com detector por ionização em chama (CG-DIC). Foram analisados três tipos de leira. Boas linearidades e coeficientes de correlação foram obtidas para todos os ácidos, e os limites de detecção e quantificação foram baixos, resultando em um método sensível para monitoramento desses ácidos em composto de RSU.

Gerenciamento de resíduos químicos em um laboratório de ensino e pesquisa: a experiência do Laboratório de Limnologia da UFRJ

This work describes the waste management system developed at the Laboratory of Limnology of Federal University of Rio de Janeiro. The initial challenge was to identify and treat a great variety of wastes generated in the analytical procedures performed in the laboratory. Since many of the students and researchers are not chemists, an intensive training was performed during the establishment of the management system. After three years, there was a deep change of attitude of the professionals involved. The present experience may be useful for other laboratories with a profile similar to the one under study.