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Fusarium graminearum and Fusarium meridionale are primary contaminants of barley, capable of producing several mycotoxins, mainly type B trichothecenes and zearalenone. Cold plasma decontamination has been gaining prominence, seeking to control the fungal and mycotoxin contamination of food and feed and to improve product quality. To reach this objective, the present study was divided into two parts. In the first part, F. meridionale and F. graminearum strains were exposed to gliding arc plasma jet (GAPJ). Cell viability tests showed the inactivation of F. meridionale after 15-min treatment, whereas F. graminearum showed to be resistant. In the second part, barley grains were treated by GAPJ for 10, 20, and 30 min, demonstrating a reduction of about 2 log CFU/g of the barley’s mycobiota, composed of yeasts, strains belonging to the F. graminearum species complex, Alternaria, and Aspergillus. A decrease in DON levels (up to 89%) was observed after exposure for 20 min. However, an increase in the toxin Deoxynivalenol-3-glucoside (D3G) was observed in barley grains, indicating a conversion of DON to D3G.

Exclusive breastfeeding is recommended for newborns until at least the sixth month. However, in some cases, the use of infant formulas as breast milk replacement has been used to provide the nutritional needs of infants. For children over six months baby foods can often be incorporated into the diet. Aluminium (Al) could be present in baby foods and it has potential neurotoxic effects when ingested and absorbed by the organism. In this study, we reviewed Al toxicology, total content and bioaccessibility in several baby food products. The study was performed as a systematic review of scientific literature on the databases Scopus, Science Direct, Web of Science, and Academic Google. Aluminium content varied according to distinct types of baby foods (0.92−2860 mg kg−1). Different analytical methods used to evaluate Al bioaccessibility, including sample preparation and in vitro conditions to simulate the gastrointestinal digestion, indicated that the Al bioaccessible fraction varied from 0.5–48% in the current literature.

Tetracyclines and polyether ionophores are veterinary drugs frequently used in animals reared for food production. Despite the benefits, residues can be harmful for human health if levels are higher than those considered safe. The aim of this study was to evaluate, by LC-MS/MS, tetracyclines residues in pasteurised milk samples marketed in São Paulo state, Brazil and estimate the exposure of the adult/adolescent/children population. Within the eight antibiotics monitored two were detected, tetracycline and 4-epitetracycline, found in 22.5% and 12.5% of the samples, respectively. Since the same samples had been previously tested for polyether ionophore residues, risk assessment based on dietary exposure to tetracyclines when considered individually and in combination with the ionophores was performed. The daily intakes were below the acceptable daily intake (ADI) for tetracycline. Considering the levels of monensin reported in a previous study, the combined exposure with tetracycline and 4-epi-tetracycline also indicated low potential health concerns.

An analytical method was developed and validated for the determination of three polyether ionophores (monensin, lasalocid, and salinomycin) in 60 samples of Brazilian Minas Frescal cheese by UHPLC-MS/MS. Linearity ranged from 1 to 8 μg kg

Inorganic contaminants, including those commonly known as ‘heavy metals’ (cadmium, arsenic, lead and mercury) and others like aluminum, copper, zinc, and nickel, may be present in baby foods such as infant formulas, cereals, snacks, prepared meals, and jarred fruits and vegetables. Children, babies and toddlers are more vulnerable to these toxic elements due to their immature development and high ‘food intake/body weight’ ratio. The most important adverse effects of inorganic contaminants for infants include: anemia, nephrotoxicity, developmental, and reproductive toxicity, lower intelligence quotient (IQ), and neurotoxic effects. As this topic represents a relevant food safety issue, this article aims to review recent data about the occurrence of inorganic contaminants in baby foods, regulatory aspects, exposure assessment, as well as analytical methods for their determination. The available information reinforces the importance of standardizing routine quality control and reducing inorganic contaminants levels in infant formula and baby foods.

3-MCPDE (3-monochloropropane-1,2-diol esters), 2-MCPDE (2-monochloropropane-1,3-diol esters) and GE (glycidyl esters) are heat-induced contaminants that are formed during the refining of vegetable oils under high temperatures, mainly during the deodorization step. Samples commercialized as extra virgin olive oils (EVOO), olive oils and oil blends (n = 76) were analysed for 3-MCPDE, 2-MCPDE and GE. A possible correlation with the identity and quality parameters established for olive oils was also evaluated. Concentrations of 3-MCPDE, 2-MCPDE and GE ranged from not detected to 1.16 mg/kg, not detected to 0.58 mg/kg and not detected to 1.98 mg/kg in EVOO, respectively. Samples commercialized as olive oil presented levels ranging from 0.28 to 3.77 mg/kg for 3-MCPDE, 0.17–1.91 mg/kg for 2-MCPDE and not detected to 1.88 mg/kg for GE. For oil blends, 3-MCPDE levels were from 0.18 to 0.61 mg/kg, 2-MCPDE were from not detected to 0.25 mg/kg and GE from 0.31 to 1.84 mg/kg. As the processing of EVOO does not require the use of high temperatures, these esters were not expected at quantifiable levels in these products, indicating that they were probably adulterated with the addition of some type of refined oil. According to this study, analysis of 3-MCPDE, 2-MCPDE and GE may also be used as a complementary indicator of adulteration of EVOO.

Rapadura is an artisanal candy obtained from concentrated sugarcane juice. In this study, a differentiation between South American rapadura producers has been tried using a Kurtosis-based projection pursuit analysis (kPPA) concerning essential minerals, acrylamide, moisture contents, pH, and color. These parameters revealed significant inter- and intra-country differences. Based on the employed measurements, a multivariate exploration with kPPA extracted information from rapadura even though it is a very artisanal product and was effective in separating classes, especially Brazilian and Ecuadorian rapadura, where principal component analysis failed. Moreover, ellipse confidence regions showed significant differences between non-organic and organic rapadura from Colombia and Peru in granulated form. From a chemometric point of view, the application of kPPA can be used in cases when other metrics (as based on the variance) fail and can be useful in the exploratory analysis of complex multivariate chemical data.

Miniaturized and simplified sample preparation methods with reduced consumption of chemicals and non-halogenated solvents are presented for the determination of 12 sulfonamides in baby foods. Hydrophilic interaction liquid chromatography coupled to quadrupole time-of-flight mass spectrometry was used for the identification and quantification of the compounds based on the acquisition of full spectrum at high resolution with accurate mass for precursor and its fragment ions. Three miniaturized protocols based on QuEChERS, salting-out assisted liquid-liquid extraction or low-temperature cleanup were evaluated regarding the extraction efficiency and removal capability of matrix co-extractives. All approaches achieved satisfactory recoveries (70.0-120.0%); however, the miniaturized QuEChERS distinguished by lower co-extractives content in the final extract providing lower matrix effects. Thus, the performance characteristics of the miniaturized QuEChERS were established using different matrices: beef-, egg yolk- and vegetable-based baby food or chicken- and vegetable-based baby food, in compliance with the Codex Alimentarius Commission guidelines. The target compounds were investigated in 30 commercial baby foods.

Sodium chloride (NaCl) is the most commonly used ingredient to provide salty taste to foods. However, excess sodium in the bloodstream has been associated with the development of several chronic noncommunicable diseases. In order to limit sodium intake to levels considered safe, the World Health Organization (WHO) recommends for adults a daily intake of not more than 5 g of NaCl (less than 2 g of sodium). One of the strategic actions recommended by the Pan American Health Organization (PAHO) to reduce sodium intake is reformulation of processed foods. This recommendation indicates there is an urgent need to find salt substitutes, and umami compounds have been pointed as an alternative strategy. Like salty, umami is also a basic taste and the major compound associated to umami is monosodium L‐glutamate (MSG). The available scientific data on the toxicity of MSG has been evaluated by scientific committees and regulatory agencies. The Joint FAO/WHO Expert Committee on Food Additives and the Scientific Committee on Food of the European Commission established an acceptable daily intake (ADI) not specified, which indicated that the substance offers no health risk when used as a food additive. The United States Food and Drug Administration and the Federation of American Societies for Experimental Biology classified MSG as a Generally Recognized as Safe (GRAS) substance. In this paper, an overview about salty and umami taste physiology, the potential applications of MSG use to reduce sodium content in specific industrialized foods and safety aspects of MSG as food additive are presented.

O uso de edulcorantes, substâncias capazes de conferir gosto doce aos alimentos, tem aumentado em razao das medidas que visam reduzir o consumo de acucar. Entretanto, para que esta pratica nao represente riscos a saude do consumidor, e preciso garantir que o consumo desses ingredientes nao ultrapasse sua Ingestao Diaria Aceitavel (IDA). Este projeto buscou analisar a exposicao da populacao infantil ao consumo de edulcorantes (acessulfame de potassio, aspartame, ciclamato de sodio, glicosideos de esteviol, sacarina sodica e sucralose) atraves da ingestao de alimentos e bebidas utilizando a abordagem passo-a-passo (tiered approach). O cenario mais conservador (tier 1) foi aplicado para criancas de 1 a 10 anos e mostrou que a IDA pode ser excedida para todos os edulcorantes, em diversas situacoes. Quando dados reais de consumo de alimentos e bebidas por criancas de 1 a 3 anos foram utilizados (tier 2), verificou-se que a IDA do ciclamato de sodio e dos glicosideos de esteviol pode ser extrapolada em 6% e 28% da populacao estudada, respectivamente. Os dados sugerem que uma abordagem mais refinada (tier 3) deve ser aplicada ao ciclamato de sodio e aos glicosideos de esteviol enquanto o consumo de acessulfame de potassio, aspartame, sacarina sodica e sucralose pode ser considerado seguro.

This paper aimed to survey the occurrence of six polyether ionophores (lasalocid, maduramycin, monensin, narasin, salinomycin and semduramycin) in pasteurized milk using a validated method by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). For that, 40 samples of pasteurized milk, from seven brands, collected in six locations (supermarkets, grocery stores and greengrocers) in the metropolitan region of Sao Paulo and Campinas, Sao Paulo State, Brazil, were evaluated. Sampling included whole (18), skimmed (8) and semi-skimmed (10) milk as well as lactose-free (4) products. Only monensin antibiotic residues were found in the analyzed samples. This ionophore was confirmed in 45% of the samples and quantified in 32.5% at concentrations ranging from 0.1 to 0.27 μg kg−1. The positive samples were whole or semi-skimmed milk. Considering the levels of monensin reported in the present study and data on milk consumption in Brazil, an exposure assessment indicated that the intake of this antibiotic does not represent a risk to health.

An accurate, sensitive and selective analytical method is proposed for sulfonamide residues analysis in infant formulas based on hydrophilic interaction liquid chromatography (HILIC) and quadrupole time-of-flight mass spectrometry in full scan mode. The sample preparation approach involves low-temperature lipid precipitation followed by dispersive solid-phase extraction with PSA and C18 sorbents, which was successfully optimized using Plackett-Burman design. In order to achieve high analytical sensitivity, the influence of HILIC conditions on sulfonamide ionization was investigated, such as the mobile phase composition, buffer concentration, and sample diluent for injection. The method performance characteristics, including linearity (range 5–120 µg kg–1), reliable limits of quantification (between 5 and 20 µg kg–1), recovery (72.9–109.2%) and precision (coefficient of variation values ≤ 19.8%) under repeatability and within-laboratory reproducibility conditions, were in accordance with the Codex Alimentarius Commission CAC/GL 71–2009 for quantitative analytical methods for veterinary drug residues in foods. Moreover, adequate identification of the compounds was provided with accurate mass measurement of both precursor and fragment ions in one single run. Finally, the developed method was applied to thirty-five powdered milk-based infant formula samples available in the Brazilian market.

Considering the widespread use of the antibiotic monensin (MON) in the Brazilian livestock and the possibility of residues in milk, this paper aimed to study the stability and fate of this drug during the production of Brazilian Minas Frescal cheese, its effects on milk fermentation and on the physicochemical characteristics of this product. For that, samples of raw milk were fortified with MON at three different nominal concentrations (1.0, 2.0 and 8.0 μg/kg), passed through heat treatment and used to produce Minas Frescal cheese. Pasteurization efficiency was certified by alkaline phosphatase and peroxidase enzyme tests and cheese samples were evaluated for pH, moisture and total protein and fat content. MON residues were determined by LC-MS/MS in the following steps: raw milk, heat-treated milk, whey and cheese. No significant degradation of MON due to heat treatment was observed, suggesting that the drug is resistant to high temperatures. Moreover, the residue levels quantified in cheese and whey demonstrated a concentration of this antibiotic in the curd by about 5-fold, with a small amount of MON being lost during draining. There were no significant differences (p > 0.05) considering the physicochemical parameters evaluated in cheese samples. Fermentation was also not affected by the presence of the drug. The results showed that residues of MON in milk are stable during cheese production and may be concentrated in the final product, as well as indicate the need to establish a MON safe residue level for this food commodity.

The objective of this study was to determine the total concentration and bioaccessible fraction of aluminium (Al) in 95 different baby food samples and estimate the exposure assessment. Total Al content was determined following oxidative microwave digestion by inductively coupled plasma optical emission spectrometry. An in vitro digestionmethod was optimized to evaluate the bioaccessible fraction. Total concentration and bioaccessibility varied according to the sample composition (saltypurees, fruit purees, infant drinks and petitsuisse). Petit suisse, soy-based drink and salty puree samples presented the highest total Al concentrations of 4170 μg kg−1, 2860 μg kg−1 and 2760 μg kg−1, respectively. Bioaccessiblefraction varied from 0.5%–48% according to their composition.Exposure to Al was estimated and compared with the tolerable weekly intakes currently established. The results showed that the consumption of 3 portions/day of soy-based drink along the week could represent a concern.

The aim of this work was to determine the total concentration and the effect of in vitro digestion on the bioaccessible fraction of aluminum (Al) in 35 different cereal-based baby food samples and estimate the exposure to this element considering the consumption of this product. Total Al content was determined by inductively coupled plasma optical emission spectrometry after oxidative microwave digestion. An in vitro digestion method was applied and optimized to evaluate the bioaccessible fraction. The methods performance was efficient for both approached analysis and presented limits of detection and quantitation of 53 μg kg−1 and 89 μg kg−1, respectively. Total concentration and bioaccessibility varied according to the product composition (rice, oat, wheat, barley, corn, multicereal and fruit). Multicereals and fruit-based (plum) cereals presented the highest total Al concentrations (8.82 mg kg−1 and 7.49 mg kg−1, respectively), whilst lower values were observed for corn and rice flour cereals (0.92 mg kg−1 and 1.09 mg kg−1, respectively). The bioaccessible fraction varied from 1.5% to 10.4% in the evaluated samples. Exposure to Al was estimated and compared with the Provisional Tolerable Weekly Intake (PTWI) of 2 mg kg−1 body weight. The results showed that the daily consumption of three portions of cereals contributes up to 10.48% of the PTWI, when considering the total Al concentration reported in this study.

Florfenicol is one of the most-used antimicrobial agents in global fish farming. Nevertheless, in most countries, its use is not conducted in accordance with good practices. The aim of this work was to evaluate the leaching of florfenicol from coated fish feed into the water. Analytical methods were developed and validated for the quantitation of florfenicol in medicated feed and water by UHPLC-MS/MS. Florfenicol residues in the water were quantified after 5- and 15-min exposures of the medicated feed in the water at 22 and 28 °C and at pH 4.5 and 8.0. The influence of pellet size and three coating agents (vegetable oil, carboxymethylcellulose, and low-methoxylated pectin) on the leaching of the drug was also assessed. Pellet size, coating agent, water temperature, and time of exposure significantly (p 0.05) affected florfenicol leaching, while water pH did not interfere with the leaching. Coating with vegetable oil was the most efficient method to reduce florfenicol leaching, while coating with carboxymethylcellulose presented the highest leaching (approximately 60% after 15 min at 28 °C). Thus, the coating agent has a significant effect on the florfenicol leaching rate and, consequently, on the necessary dose of the drug to be administered. Moreover, it is worth mentioning that higher florfenicol leaching will pose a greater risk to environmental health, specifically in terms of the development of bacteria resistant to florfenicol. Additional studies are needed with other polymers and veterinary drugs used in medicated feed for fish farming.

Considering the immaturity of babies’ gastrointestinal system, particularly those of newborn infants, elevated aluminum (Al) concentrations can be toxic, and exposure to this contaminant due to the substitution of breast milk by infant formulae may represent a risk. The main sources of Al contamination in these products include the variability in the raw material (milk or soy), the formula composition, the contamination during processing and the presence of additives or mineral supplements. However, there are few recent reports in the literature on the occurrence of Al in milk-based or soy-based infant formulae. Thus, the aim of the present work was to study the presence of Al in samples of infant formulae acquired on the local market in Campinas, Sao Paulo, Brazil and estimate children exposure to this element. The Al contents were determined using optical emission spectrometry with an inductively coupled plasma source. The results obtained presented maximum values of 1.46, 5.94 and 4.49 mg kg−1 for starter, follow-up and specialized formulae, respectively. As from these data, it was estimated that the consumption of infant formulae (0–6 months) could reach 22.4% of the Al tolerable weekly intake (TWI), whereas a maximum value of 29.4% was observed for children between 12–24 months. The results obtained in this study show that the Al levels in infant formulae could suggest a potential concern for infants, and should therefore be monitored.

Orientadores: Maria Cecilia de Figueiredo Toledo Tese (doutorado) Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos Resumo: Uma importante descoberta de pesquisadores suecos em abril de 2002 mostrou que acrilamida, uma substância provavelmente carcinogênica a seres humanos, pode ser formada em determinados alimentos que são submetidos a tratamento térmico em altas temperaturas. No presente estudo, 111 amostras de diferentes categorias de alimentos foram coletadas em supermercados, lojas de ¿fast-foods¿ e restaurantes da cidade de Campinas-SP, entre os meses de setembro de 2004 e abril de 2006, e analisadas para verificar a presença de acrilamida. As amostras foram selecionadas em função dos resultados divulgados por outros países e incluíram, além de produtos à base de batata, trigo e café, alimentos tipicamente brasileiros à base de mandioca e milho, processados em altas temperaturas. Os níveis de acrilamida foram determinados por cromatografia líquida de alta eficiência e espectrometria de massas em série (LC-MS/MS), conforme método previamente desenvolvido. Como a aplicação deste método em matrizes de cacau não apresentou resultados satisfatórios, o mesmo foi modificado através da inclusão de uma etapa de precipitação de proteínas e de alterações no procedimento de limpeza, o que resultou em melhor desempenho nesta matriz. As concentrações de acrilamida determinadas nas amostras analisadas confirmam que produtos à base de batata, tais como batatas fritas e batatas chips, biscoitos e café são os alimentos que apresentam os maiores níveis de acrilamida. Em etapa posterior, a ingestão potencial diária deste contaminante foi estimada combinando-se os dados analíticos de ocorrência de acrilamida obtidos no presente estudo com dados de consumo dos alimentos analisados, disponíveis para a população em geral e para uma população de adolescentes da cidade de Piracicaba-SP. Os valores médios de ingestão estimados para ambas as populações (0,14 e 0,12 µg/kg de peso corpóreo/dia, respectivamente) são inferiores aos valores relatados para populações de países da América do Norte e Europa (0,3 a 2 µg/kg de peso corpóreo/dia), o que pode ser parcialmente atribuído ao fato de que as estimativas de ingestão nestes países levaram em conta a contribuição de um maior número de alimentos. Dessa forma, é importante que mais amostras e grupos de alimentos sejam investigados para que, futuramente, possa ser calculada a contribuição da dieta total como fonte de acrilamida para a população brasileira e avaliados os possíveis riscos à saúde relacionados à exposição a este contaminante Abstract: An important discovery of Swedish researchers in April 2002 showed that acrylamide, a probable carcinogen to humans, can be formed in certain foods which are submitted to thermal treatment at high temperatures. In the present study, 111 samples of different food categories were collected at supermarkets, fast-food restaurants and restaurants, in Campinas-SP, between September 2004 and April 2006, and analysed to verify the presence of acrylamide. The samples were selected according to results reported in other countries and included, beyond potato- and wheat-based products and coffee, typical Brazilian foods made from cassava and maize, and processed at high temperatures. The levels of acrylamide were determined by high performance liquid chromatography tandem mass spectrometry (LC-MS/MS), according to a method previously developed. As the application of this method in cocoa matrices did not presented satisfactory results, there was a need to modify it by the inclusion of a protein precipitation step and changes in the clean-up procedure, which improved its performance in this matrix. The concentrations of acrylamide determined in analysed samples confirm that potato-based products, such as French fries and potato chips, biscuits and coffee are the foods containing the highest levels of acrylamide. In a next step, the potential daily intake of this contaminant was estimated by combining analytical data on the occurrence of acrylamide obtained in the present study with data on food consumption for the analysed foods, available for the general population and for a population of adolescents from the city of Piracicaba-SP. The mean intakes estimated for both populations (0.14 e 0.12 µg/kg body weight/day, respectively) are below the values reported for populations from North American and European countries (0.3 to 2 µg/kg body weight/day), which may be partially attributed to the fact that intake estimates conducted in these countries took into account the contribution of a greater number of foods. In this way, it is important that more samples and food groups be investigated so that, in the future, it may be possible to calculate the contribution of the total diet as source of acrylamide for the Brazilian population, and to assess the possible risks to health with regard to the exposure to this contaminant Doutorado Doutor em Ciência de Alimentos

Orientador: Marise Aparecida Rodrigues Pollonio Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos Resumo: A primeira parte deste trabalho avaliou a aceitação global de uma formulação desenvolvida para hambúrguer tipo calabresa a partir de carne suína como matéria-prima principal e a possível redução do nível de nitrito utilizado através de análise sensorial. Foram investigados também algumas características químicas (umidade, proteínas, lipídeos, cinzas e nitrito residual) de quatro formulações com diferentes níveis de nitrito e conteúdos de gordura. Na segunda parte, foram estudados os efeitos da redução do nível de nitrito de 150 para 50 mg de nitrito/Kg de produto e do conteúdo de gordura de 20 para 10% sobre a qualidade global do produto durante 120 dias de estocagem congelada. A qualidade sensorial, medida através da aparência, sabor, aroma e textura, a cor objetiva e a estabilidade oxidativa, medida através do número de substâncias reativas ao ácido 2-tiobarbitúrico (TBARS) e dos atributos sabor oxidado e aroma oxidado, foram determinadas nos tempos zero, 30, 60, 90 e 120 dias após o processamento. A cor e o número de TBARS foram determinados nas amostras cruas e cozidas. Os resultados obtidos na primeira parte indicaram que os consumidores aprovaram o novo produto e que é possível reduzir o nível de nitrito de 150 para 50 mg de nitrito/Kg de produto sem que se percam as características organolépticas de um produto curado. Após o processamento e o tratamento térmico, aproximadamente 34% do nitrito inicialmente adicionado pôde ser detectado nas amostras. Na segunda parte do trabalho, verificou-se que a redução do nível de nitrito não provocou alterações significativas entre os tratamentos para os atributos aparência, sabor, aroma e textura e para os parâmetros L*, a* e b* das amostras cruas e L* e b* das amostras cozidas. O valor a* das amostras cozidas geralmente foi maior para as amostras com mais nitrito. No estudo de estabilidade oxidativa observou-se que 50 mg de nitrito/Kg de produto exerceu um bom efeito antioxidante até 30 dias. Com 60 dias, amostras cozidas que continham inicialmente 150 mg de nitrito/Kg de produto, mostraram-se menos oxidadas, com menores valores de TBARS. A redução no conteúdo de gordura não afetou as propriedades sensoriais ao longo do período de estocagem congelada, mas exerceu um forte efeito sobre os parâmetros L* e a* das amostras cruas. Amostras com 20% de gordura foram mais claras e menos vermelhas enquanto amostras com 10% de gordura foram mais escuras e mais vermelhas. Nas amostras cozidas, a redução do teor de gordura não exerceu efeito significativo sobre os parâmetros L*, a* e b*. Os tratamentos com maior % de gordura apresentaram maiores valores de TBARS em 90 e 120 dias para as amostras cozidas. Com relação à estabilidade durante a estocagem, todas as formulações apresentaram atributos sensoriais (aparência, sabor, aroma e textura) satisfatórios. O parâmetro L * diminuiu significativamente tanto nas amostras cruas quanto nas cozidas, o valor a* sofreu alteração durante a estocagem somente nas amostras cozidas dos tratamentos com 50 mg de nitrito/Kg de produto e 20% de gordura e com 150 mg de nitrito/Kg de produto e 10% de gordura e, para o valor b*, observou-se uma redução ao longo dos 120 dias de estocagem congelada para as amostras cruas de todos os tratamentos. O valor de TBARS aumentou significativamente com o tempo nas amostras cruas e cozidas de todos os tratamentos, sendo que esse aumento foi mais significativo após 30 dias de estocagem congelada. O cozimento não alterou de modo significativo o valor de TBARS das amostras e foram encontrados correlações significativas positivas entre os dados de TBARS e análise sensorial para o atributo sabor oxidado considerando-se todos os pares de dados (r=0,6398) e dados entre tempos para cada tratamento (somente para as amostras com 10% de gordura) Abstract: The first part of this work investigated a developed formulation for a new meat product, denominated "calabresa" sausage - style hamburger from pork meat. The overall acceptability and the possible nitrite levels reduction were evaluated through sensory analysis. The chemical composition and residual nitrite were also determined. The second part of this research studied the effects of nitrite levels reduction from 150 mg/Kg to 50 mg/Kg and the fat content reduction from 20% to 10% on product overall quality during frozen storage The sensory characteristics like appearance, taste, smell and texture, the objective color and oxidative stability were determined at day O, 30, 60, 90 and 120 days after processing. The first part results have indicated that consumers approved the new product and the nitrite levels reduction from 150 to 50 mg/Kg is possible without losses of cured meat characteristics. After processing and thermal treatment, only 34% of the ingoing nitrite was detected. The second part results verified that the sensory properties and L*, a* and b* parameters of raw hamburgers and L* and b* of cooked hamburgers were not affected by the changes in nitrite level. In general, cooked samples with 150 mg/Kg nitrite had highest values a*. During 30 days, 50 mg/Kg nitrite showed to be a good antioxidant. With 60 days, cooked samples (150 mg/Kg nitrite) showed the lowest TBARS (2-thiobarbituric acid reactive substances) values. The fat content reduction had a strong effect on color (L* and a* values) of the raw hamburgers during frozen storage, but the sensory properties were not affected. Treatments with 20% fat were lighter and least red whereas the treatments with 10% fat were darker and redder. The L*, a* and b* parameters of cooked samples were not significantly affected by the changes in fat content. Formulations with 20% fat showed the highest TBARS values at 90 and 120 days for cooked samples. Regarding product stability during frozen sterage, all formulations showed satisfactory sensory attributes. The lightness (L *) decreased as much in the raw hamburgers as in the cooked hamburgers, the redness (a*) was affected in the cooked samples of 2 treatments (50 mg/Kg nitrite, 20% fat and 150 mg/Kg nitrite, 10% fat) and the yellowness (b*) was reduced along 120 days for raw samples. The TBARS values had a significantly increase, more intense after 30 days in raw and cooked samples and were not affected by cooking. Significant correlations were found between TBARS values and sensory analysis only for oxidized taste pooling information within treatments and storage times (r=O,6398) and within time (only for treatments of 10% fat) Mestrado Engenharia de Alimentos Mestre em Tecnologia de Alimentos

O benzoato de emamectina, um antiparasitário da classe das avermectinas, é amplamente utilizado em diversos países para o tratamento de infecções causadas por helmintos intestinais e ectoparasitas, os quais estão relacionados a grandes prejuízos na produção aquícola. Apesar de sua eficácia ser conhecida na aquicultura, seu uso não está regulamentado no Brasil. Diante da demanda nacional por uma maior variedade de medicamentos veterinários regulamentados para uso em espécies aquícolas, o presente projeto visou estimar um período de carência para o antiparasitário benzoato de emamectina, a partir de um estudo experimental de depleção residual desse fármaco em tilápia (filé com pele em proporção natural), a espécie de maior importância comercial para a produção aquícola no Brasil. Para tanto, fez-se necessárias as seguintes etapas: (i) incorporar o benzoato de emamectina na ração através da técnica de revestimento polimérico em equipamento de leito fluidizado; (ii) desenvolver e validar métodos analíticos para a determinação do benzoato de emamectina na ração e em filé de tilápia empregando cromatografia líquida de alta eficiência acoplada à espectrometria de massas (LC- MS/MS); e (iii) realizar um ensaio com tilápias para avaliar a depleção residual de emamectina B1a no filé. O revestimento da ração com 1,5% de etilcelulose permitiu incorporar o benzoato de emaectina na ração sem alterar a estrutura física da mesma, o que torna o processo vantajoso, visto que a ração mantém suas características nutricionais e de flutuabilidade. Além disso, o processo foi homogêneo (CV de 2,1%) e não apresentou taxa de lixiviação quantificável do fármaco para a água, contribuindo para uma maior segurança em relação à dose de tratamento a ser administrada e em relação ao risco potencial ao meio ambiente. A emamectina B1a foi extraída da ração por processo sólido-líquido e do filé de tilápia pelo método QuEChERS modificado. Os métodos foram avaliados mediante os seguintes parâmetros: seletividade, curva analítica, linearidade, precisão, exatidão, limite de detecção (LD) e de quantificação (LQ). Todos os parâmetros avaliados se encontraram conformes às recomendações dos guias de validação tomados como referências, qualificando os métodos como adequados para os objetivos propostos no presente trabalho. Para avaliar a depleção de emamectina B1a no filé de tilápia, os peixes receberam o fármaco via ração em dose de 50 ?g/kgPV/dia durante sete dias consecutivos. As curvas de depleção residual de emamectina B1a se ajustaram ao modelo exponencial de primeira ordem. Tomando como referência o limite máximo de resíduo de 100 ?g/kg recomendado pelo Codex Alimentarius, não houve a necessidade de se propor um período de carência mínimo para o abate dos peixes, considerando as condições experimentais empregadas. Emamectin benzoate, an antiparasitic of the class of avermectins, it is widely used in several countries for the treatment of infections caused by intestinal helminths and ectoparasites, which are related to great losses in aquaculture production. Although its known effectiveness for aquaculture, its use is not regulated in Brazil. The national demand for a greater variety of regulated veterinary drugs for use in aquaculture species,the current project that aimed to evaluate a withdrawal period for the antiparasitic emamectin benzoate, based on an experimental study of residual depletion of this drug in tilapia ( fillet with skin in natural proportion) the species of major commercial importance for aquaculture production in Brazil. To do so, it was necessary to: (i) incorporate emamectin benzoate into the feed through the polymer coating technique in fluidized bed equipment; (ii) to develop and validate the analytical methods for the determination of emamectin benzoate in the feed and in tilapia fillet using high-performance liquid chromatography coupled to mass spectrometry (LC-MS / MS) and (iii) perform a tilapia test to evaluate the depletion of emamectin B1a in fillet. The feed coating with 1.5% ethylcellulose allowed to incorporate the emaectin benzoate into the feed without altering the physical structure, which makes the process advantageous, since the feed retains its nutritional and buoyancy characteristics. In addition, the process was homogeneous (CV 2,1%) and did not present quantifiable leaching rate of the drug into the water, contributing to a greater safety in relation to the dose of treatment to be administered and in relation to potential risk to the environment. Emamectin B1a was extracted from the feed by solid-liquid process and from tilapia fillet by the modified QuEChERS method. The methods were evaluated using the following parameters: selectivity, analytical curve, linearity, precision, accuracy, limit of detection (LD) and quantification (LQ). All the evaluated parameters were in accordance with the recommendations of the validation guides taken as references, qualifying the methods as adequate for the objectives proposed in the present work. To evaluate the depletion of emamectin B1a tilapia fillet, the fish received the drug via feed at a dose of 50 ?g / kgPV / day for seven consecutive days. The residual depletion curves of emamectin B1a were fitted to the first order exponential model. Taking into account the maximum residue limit of 100 ?g / kg recommended by the Codex Alimentarius, there was no need to propose a minimum withdrawal period for the slaughtering of fish, considering the experimental conditions used.

Introdução: A alimentação na atualidade está relacionada a questões de saúde pública, por ser um dos fatores que contribuem com a incidência das doenças crônicas não transmissíveis, dentre elas, a hipertensão. O consumo excessivo de sódio está associado a vários efeitos prejudiciais à saúde, como o aumento da pressão arterial e doença cardiovascular. De acordo com a Organização Mundial da Saúde (OMS), o consumo diário de sódio não deveria ultrapassar 2,0g/pessoa/dia, por causa do aumento do risco de desenvolvimento de doenças crônicas não transmissíveis. Dados da última Pesquisa de Orçamentos Familiares mostram que os brasileiros consomem, em média, 4,7g/pessoa/dia, ou seja, mais que o dobro da recomendação da OMS. Objetivo: Verificar se o gosto básico umami, na forma de glutamato monossódico monoidratado, é uma alternativa para a redução de sódio no preparo das refeições. Metodologia: Foi realizado pré-teste para definir a concentração de MSG e sal a ser utilizada nas preparações. A quantidade para o arroz com sal foi de 1,08% de adição e para o arroz com sal e MSG foi de 0,54% e 0,43% respectivamente. Para a carne com sal adicionou-se 1,10% de sal e para a carne com sal e MSG foi adicionado 0,55% e 0,44%, respectivamente. Uma amostra de arroz e de carne sem sal e sem MSG também foi preparada. Houve a apresentação a um vídeo como variável comportamental sobre adição de sal e saúde. Foi realizada análise sensorial - teste de preferência entre as 3 amostras de arroz e 3 de carne bovina - e análises físico-químicas para avaliar as quantidades de sódio e de ácido glutâmico nas amostras. A análise estatística dos resultados obtidos foi realizada por análise de variância ANOVA e teste de Friedman- valores de amplitude total estudentizada (q) /nota: nível em 5% de probabilidade. Também foram realizados cálculos dos valores de médias, desvio padrão, gráficos de distribuição, máximos e mínimos. As análises foram realizadas utilizando os softwares Microsoft Excel 2010, Stata12.0 e FizzBiosystemes®. Resultados: Participaram dos testes 103 indivíduos de ambos os gêneros, com idade entre 18 e 57 anos, sendo que 52 assistiram ao vídeo e 51 não. Os resultados demonstraram que não houve diferença significativa entre assistir ou não ao vídeo no comportamento de intenção de adição de sal às preparações pelos provadores. Os testes de preferência das preparações do arroz e da carne não apresentaram diferença significativa entre as amostras preparadas apenas com sal àquelas preparadas com sal e MSG (p>0,05). Comparando as amostras de arroz com sal e de arroz com sal e MSG o resultado obtido na análise físico química foi de 30,2% de redução de sódio. Comparando as amostras de carne com sal e de carne com sal e MSG, o resultado obtido foi de 33,12% de redução de sódio. A carne bovina contem naturalmente ácido glutâmico livre (18 mg/100g), possuindo também inosinato (80 mg/100g), o que potencializa o gosto umami naturalmente presente no alimento. Assim, por ser saborosa é possível reduzir mais o sódio quando comparada ao arroz, o qual possui naturalmente apenas 5,86mg de ácido glutâmico/100g, não apresentando quantidades significativas de inosinato. Conclusão: O MSG, que possui as propriedades gustativas do umami, pode ser um coadjuvante para reduzir a ingestão de sódio, conforme ficou evidenciado nos resultados do presente estudo. Introduction: Current nutrition is related to public health issues, since it is one of the factors that contribute to the incidence of chronic non-communicable diseases, among them, hypertension. Excessive sodium intake is associated with several detrimental health effects, such as increased blood pressure and cardiovascular disease. According to the World Health Organization (WHO), daily sodium intake should not exceed 2.0g / person / day because of the increased risk of developing non-communicable chronic diseases. Data from the last Family Budget Survey show that Brazilians consume, on average, 4.7 g / person / day, that is, more than twice the WHO recommendation. Objective: To verify if the basic taste umami, in the form of monosodium glutamate monohydrate, is efficient in reducing sodium in the meal preparations. Methodology: A pre-test was performed to define the concentration of MSG and salt to be used in the preparations. The amount of salt added in plain rice was 1.08%. For rice with salt and MSG was added 0.54% of salt and 0.43% of MSG. To prepare meat with salt, 1.10% of salt was added. To prepare meat with salt and MSG, 0.55% of salt and 0.44% of MSG were added. A sample of rice and meat without salt and no MSG was also prepared. A video about addition of salt and its impact on health was prepared as a behavioural variable. Sensory analysis - preference test between the 3 rice and 3 beef samples - and physical-chemical analyses were performed to evaluate the amounts of sodium and glutamic acid in the samples. Statistical analysis of the results was performed by analysis of variance ANOVA and Friedman test - values of total amplitude studentized (q) / note: level in 5% of probability. Were also performed calculations of averages, standard deviation, distribution and maximum and minimum values. Analyses were performed using the software Microsoft Excel 2010, Stata12.0 and FizzBiosystemes®. Results: A total of 103 individuals from both genders, aged between 18 and 57 years old, participated in the tests, 52 of them watched the video and 51 did not. The results showed that there was no significant effect of video watching on the intention of adding salt to the preparations. Preference tests for both rice and meat preparations showed no significant difference between the salt-only samples and those prepared with MSG (p> 0.05). When comparing the samples of rice with salt alone and rice with salt and MSG, the result obtained in the physical chemical analysis was 30.2% of sodium reduction. Comparing the samples of meat with salt alone and meat with salt and MSG, the result was 33.12% of sodium reduction. Beef naturally contains free glutamic acid (18 mg / 100 g) and inosinate (80 mg / 100 g), which potentiates the naturally occurring umami taste in the food. Thus, we hypothesize that because beef is umami-rich, it is possible to reduce sodium more than in rice, which naturally contains only 5.86 mg of glutamic acid / 100 g, and does not contain significant amounts of inosinate. Conclusion: MSG, which is the principal signal of umami taste, can be a cooking tool to reduce sodium intake, as evidenced in the results of the present study.