Desenvolvimento de métodos para quantificação de benzilpenicilina em medicamentos veterinários e seus resíduos em leite bovino e caprino por UFLC-DAD

The Benzylpenicillin (PENG) have been as the active ingredient in veterinary medicinal products, to increase productivity, due to its therapeutic properties. However, one of unfortunate quality and used indiscriminately, resulting in residues in foods exposed to human consumption, especially in milk that is essential to the diet of children and the ageing. Thus, it is indispensable to develop new methods able to detect this waste food, at levels that are toxic to human health, in order to contribute to the food security of consumers and collaborate with regulatory agencies in an efficient inspection. In this work, were developed methods for the quality control of veterinary drugs based on Benzylpenicillin (PENG) that are used in livestock production. Additionally, were validated methodologies for identifying and quantifying the antibiotic residues in milk bovine and caprine. For this, the analytical control was performed two steps. At first, the groups of samples of medicinal products I, II, III, IV and V, individually, were characterized by medium infrared spectroscopy (4000 – 600 cm-1). Besides, 37 samples, distributed in these groups, were analyzed by spectroscopy in the ultraviolet and near infrared region (UV VIS NIR) and Ultra Fast Liquid Chromatograph coupled to linear arrangement photodiodes (UFLC-DAD). The results of the characterization indicated similarities, between PENG and reference standard samples, primarily in regions of 1818 to 1724 cm-1 of ν C=O that shows primary amides features of PENG. The method by UFLC-DAD presented R on 0.9991. LOD of 7.384 × 10-4 μg mL-1. LOQ of 2.049 × 10-3 μg mL-1. The analysis shows that 62.16% the samples presented purity ≥ 81.21%. The method by spectroscopy in the UV VIS NIR presented medium error ≤ 8 – 12% between the reference and experimental criteria, indicating is a secure choice for rapid determination of PENG. In the second stage, was acquiring a method for the extraction and isolation of PENG by the addition of buffer McIlvaine, used for precipitation of proteins total, at pH 4.0. The results showed excellent recovery values PENG, being close to 92.05% of samples of bovine milk (method 1). While samples of milk goats (method 2) the recovery of PENG were 95.83%. The methods for UFLC-DAD have been validated in accordance with the maximum residue limit (LMR) of 4 μg Kg-1 standardized by CAC/GL16. Validation of the method 1 indicated R by 0.9975. LOD of 7.246 × 10-4 μg mL-1. LOQ de 2.196 × 10-3 μg mL-1. The application of the method 1 showed that 12% the samples presented concentration of residues of PENG > LMR. The method 2 indicated R by 0.9995. LOD 8.251 × 10-4 μg mL-1. LOQ de 2.5270 × 10-3 μg mL-1. The application of the method showed that 15% of the samples were above the tolerable. The comparative analysis between the methods pointed better validation for LCP samples, because the reduction of the matrix effect, on this account the tcalculs < ttable, caused by the increase of recovery of the PENG. In this mode, all the operations developed to deliver simplicity, speed, selectivity, reduced analysis time and reagent use and toxic solvents, particularly if compared to the established methodologies.

Investigação da rota biohidrometalúrgica com Acidithiobacillus ferrooxidans/thiooxidans para recuperação do cobalto de baterias de íons lítio descartadas

The recycling of metals from secondary sources can be advantageous. Among the metals of interest, we have cobalt, a metal used for various purposes. As regards the secondary sources of cobalt, the lithium-ion batteries can be considered, since they contain cobalt oxide in their composition (LiCoO2). This way, the objective of this work was to use the microorganism strains (Acidithiobacillus ferrooxidans and Acidithiobacillus thiooxidans) to bioleach the LiCoO2 extracted from discarded lithium ion batteries with emphasis on the recovery of cobalt for synthesis of new materials of interest. The lineage growth occurred in T&K medium and the growth investigation was made by observing the media, by platelet growth and microscope analysis. Then, the inoculum was standardized on 5 x 106 cells mL-1 and used in bioleaching tests. The bioleaching was investigated: the microorganism nature: separate strains and A. ferrooxidans and A. thiooxidans consortium, bioleaching time (0 to 40 days), inoculum proportion (5 to 50% v/v), energy source (iron and sulfur) and residue concentration (1063 to 8500 mg L-1 of cobalt). The cobalt concentration in the media was found by atomic absorption spectrometry and the medium pH was monitored during the bioleaching. The results show that the amount of bioleached cobalt increases with time and the iron concentration. The bioleaching with A. thiooxidans was not influenced by the addition of sulfur. The use of the two lineages together did not improve the bioleaching rates. Among the lineages, the A. thiooxidans presented better results and was able to bioleach cobalt amounts above 50% in most of the experiments. A. thiooxidans presented lower bioleaching rates, with a maximum of 50% after 24 days of experiment. After reprocessing by bioleaching, the cobalt in solution was used for synthesis of new materials: such as LiCoO2 cathode and as adsorbent pesticide double lamellar hydroxide (HDL Co-Al-Cl) by the Pechini and co-precipitation methods. The reprocessed LiCoO2 presented a unique stoichiometric phase relative to the HT-LiCoO2 structure similar to the JCPDS 44-0145, presenting electrochemical activity when tested as a cathode material. The double lamellar hydroxide Co-Al-Cl was tested as pesticide adsorbent, being possible to adsorb around 100% of the pesticide. The bioleaching was efficient in the recovery of cobalt present in lithium-ion batteries and microorganisms presented high tolerance to the residue, being able to bioleach even at higher LiCoO2 concentrations. The cobalt bioleaching medium did not impair the synthesis phases and the obtained materials presented structure and activity similar to the sintered materials from the reagents containing cobalt.

Intervenção socioeducativa: investigação-ação participativa com trabalhadoras do sexo de rua e uma equipa de outreach

Nos últimos anos, assistimos ao crescimento do conhecimento sobre o trabalho sexual e os seus atores. No entanto, poucos estudos envolvem os/as trabalhadores/as do sexo (TS) como participantes ativos. Esta tese apresenta uma pesquisa de investigação-ação participativa (IAP) composta por dois estudos que, de forma complementar, pretendem contribuir para o desenvolvimento de uma proposta socioeducativa de intervenção centrada nos direitos e necessidades dos/as TS. O estudo preliminar pretende refletir sobre os discursos institucionais produzidos em torno do trabalho sexual e dar a conhecer as práticas socioeducativas empreendidas pelas instituições que dirigem serviços a TS, em Portugal. O segundo estudo apresenta o processo e os resultados de uma IAP, com TS de rua e uma equipa de outreach. O propósito do segundo estudo consistiu em identificar as necessidades e as vontades das TS e de uma equipa de outreach, com a finalidade de encorajar os/as participantes na construção de um modelo socioeducativo de intervenção. O estudo preliminar foi efetuado junto das 23 instituições que, à data deste estudo (de outubro de 2012 a março de 2013), prestavam apoio a TS. Concluímos que os serviços são bastante similares, focados na redução de riscos decorrentes do trabalho sexual, sobretudo a nível da promoção e educação para a saúde, assumindo uma intervenção tradicional centrada na epidemiologia. De forma menos expressiva, encontrámos instituições que se centram no apoio ao abandono da atividade. Todas assumem um papel fundamental no debate social e político sobre a prostituição enquanto trabalho ou opressão. Estes resultados conduziram-nos à formulação das seguintes questões: 1) Os serviços tradicionais centrados na epidemiologia reforçam inadvertidamente o estigma do/a TS?; 2) Quais são as preocupações, necessidades e vontades reais dos/as TS?; 3) O que pensam sobre serem envolvidos/as no desenho, implementação e avaliação de projetos que lhes dizem respeito? Assim, identificámos uma falta de participação dos/as TS em projetos a si dirigidos, corroborada pela literatura científica. O segundo estudo foi desenvolvido, de setembro de 2012 a junho de 2015, através de três ciclos de planificação-ação-reflexão com TS de rua e uma equipa de outreach, em Coimbra, tendo envolvido 28 participantes formais. Através de entrevistas e da reinterpretação conjunta dos resultados das mesmas, verificámos a existência de preocupações comuns, designadamente no que se refere à saúde e segurança ocupacionais, mas pouca coesão entre as TS. As iniciativas de conscientização, desenvolvidas no âmbito da IAP, providenciaram um sentido de controlo, mas a transformação da subjetividade em ação coletiva continua a ser premente. Por tal, propomos um modelo de intervenção socioeducativa com TS, segundo uma abordagem centrada na relação e na prática reflexiva, através do recurso a métodos e à filosofia da IAP. Propomos, ainda, algumas recomendações em torno da educação/formação dos profissionais de proximidade, das/os TS e, a um nível macro, iniciativas educativas centrada na desconstrução social do género.

A autorregulação aplicada aos métodos de estudo

Relatório de Estágio apresentado à Escola Superior de Educação de Lisboa para obtenção de grau de mestre em Ensino do 1.º e 2.º Ciclos do Ensino Básico

A investigação-ação e suas modalidades

O presente Manual inscreve-se no quadro de uma pedagogia que considera a iniciação à investigação como um elemento fundamental do processo de ensino/aprendizagem, determinante para a motivação dos alunos e, ao mesmo tempo, garantia da renovação do saber e da descoberta de respostas para os desafios e interrogações do futuro. Podemos apontar como intenção primeira, suscitar no leitor uma compreensão efectiva da natureza, objectivos, métodos e resultados da investigação qualitativa, mediante informação suficiente, rigorosa, actualizada e crítica. Nesse sentido não deixamos de colocar o leitor, ainda que de modo breve e introdutório, perante os fundamentos epistemológicos que subjazem a uma opção pela investigação qualitativa. E uma vez que a nossa proposta se dirige, muito em especial, à investigação do fenómeno educativo, quisemos partir, também, de uma visão complexa desse mesmo fenómeno. Enfim, apostámos na construção de um texto que ajude os seus leitores a empenharem-se num processo investigativo de natureza qualitativa, através do desenho de um plano de investigação adequado ao problema formulado (em termos de estratégia geral, de técnicas de recolha e de análise de dados), e que patenteie preocupação pela validação da mesma e pelos aspetos éticos em jogo.

A importância da análise da informação criminal para a investigação: O contributo dos NAIIC

Ao longo dos anos a Guarda Nacional Republicana tem vindo a desenvolver o seu modelo de investigação criminal. Alicerçado em três vertentes funcionais: operativa, criminalística e análise de informação criminal, este modelo visa garantir uma eficácia operacional da Guarda, no âmbito das competências que lhe são atribuídas enquanto Órgão de Polícia Criminal. Perspetivando uma evolução da investigação criminal exercida pelos Comandos Territoriais, assente numa avaliação da vertente de análise de informação criminal, surge a presente investigação, subordinada ao tema “A Importância da Análise de Informação Criminal para a Investigação: o Contributo dos NAIIC”. Com o objetivo de compreender qual o contributo que os Núcleos de Análise de Informações e Informação Criminal dos Comandos Territoriais conferem às investigações, apoiamo-nos num processo indutivo, que intenta generalizar os problemas observados nos vários Núcleos, para caracterizar a vertente de análise de informação criminal no dispositivo territorial. Visando uma análise quantitativa e qualitativa dos resultados, os métodos de recolha de dados explorados foram: dois inquéritos por questionário, um direcionado aos Chefes dos Núcleos de Análise de Informações e Informação Criminal e outro aos Chefes dos Núcleos de Investigação Criminal dos Comandos e Destacamentos Territoriais, assim como um inquérito por entrevista, realizado a cinco Oficiais da Guarda, com reconhecidos conhecimentos e experiência profissional nesta área. Conclui-se que os Núcleos de Análise de Informações e Informação Criminal têm contribuído para as investigações, enfatizando os aspetos relevantes de grandes volumes de informação, com vista a apoiar a ação dos investigadores. Todavia, foram observadas algumas limitações que importa suprimir, de forma a potenciar este contributo. Foram identificadas nestes Núcleos, insuficiências nos acessos à informação, lacunas nas ferramentas de análise, reduzido efetivo em determinados Comandos e algumas falhas de cooperação e coordenação, entre estes e os Núcleos de Investigação Criminal.

Detecção de Salmonella em tomates (Lycopersicon esculentum mill) pelos métodos fda-bam e mini vidas-biomérieux.

Resumo: Diversos surtos de Salmonella ocasionados pelo consumo de tomate contaminados com este micro-organismo têm sido relatados ultimamente, o que torna primordial a investigação sobre a presença desse patógeno nesse alimento. Métodos que permitam a avaliação rápida da presença de Salmonella em alimentos são de suma importância. O objetivo desse estudo foi comparar o método tradicional da Food and Drug Administration - Bacteriologycal Analytical Manual (FDA-BAM) com um método rápido da mini Vitek Immuno Diagnostic System Assay (Mini?Vidas-SLM)-bioMérieux, para detecção de Salmonella Brazil inoculada artificialmente na superfície de tomates. Foram analisadas 215 amostras de tomates inoculadas artificialmente com Salmonella Brazil com níveis de inóculos variando de 0,4 a 940 UFC/tomate. Os resultados obtidos mostraram que os métodos estudados apresentaram uma ótima concordância entre si, para todas as faixas de inóculo analisadas.

Espécies reativas de oxigênio e de nitrogênio, antioxidantes e marcadores de dano oxidativo em sangue humano: principais métodos analíticos para sua determinação

We review here the chemistry of reactive oxygen and nitrogen species, their biological sources and targets; particularly, biomolecules implicated in the redox balance of the human blood, and appraise the analytical methods available for their detection and quantification. Those biomolecules are represented by the enzymatic antioxidant defense machinery, whereas coadjutant reducing protection is provided by several low molecular weight molecules. Biomolecules can be injured by RONS yielding a large repertoire of oxidized products, some of which can be taken as biomarkers of oxidative damage. Their reliable determination is of utmost interest for their potentiality in diagnosis, prevention and treatment of maladies.

Aplicação de métodos de calibração multivariada para a determinação simultânea de riboflavina (VB2), tiamina (VB1), piridoxina (VB6) e nicotinamida (VPP)

In this work, the artificial neural networks (ANN) and partial least squares (PLS) regression were applied to UV spectral data for quantitative determination of thiamin hydrochloride (VB1), riboflavin phosphate (VB2), pyridoxine hydrochloride (VB6) and nicotinamide (VPP) in pharmaceutical samples. For calibration purposes, commercial samples in 0.2 mol L-1 acetate buffer (pH 4.0) were employed as standards. The concentration ranges used in the calibration step were: 0.1 - 7.5 mg L-1 for VB1, 0.1 - 3.0 mg L-1 for VB2, 0.1 - 3.0 mg L-1 for VB6 and 0.4 - 30.0 mg L-1 for VPP. From the results it is possible to verify that both methods can be successfully applied for these determinations. The similar error values were obtained by using neural network or PLS methods. The proposed methodology is simple, rapid and can be easily used in quality control laboratories.

Química forense: perspectivas sobre novos métodos analíticos aplicados à documentoscopia, balística e drogas de abuso

In this review recent methods developed and applied to solve criminal occurences related to documentoscopy, ballistic and drugs of abuse are discussed. In documentoscopy, aging of ink writings, the sequence of line crossings and counterfeiting of documents are aspects to be solved with reproducible, fast and non-destructive methods. In ballistic, the industries are currently producing ''lead-free'' or ''nontoxic'' handgun ammunitions, so new methods of gunshot residues characterization are being presented. For drugs analysis, easy ambient sonic-spray ionization mass spectrometry (EASI-MS) is shown to provide a relatively simple and selective screening tool to distinguish m-CPP and amphetamines (MDMA) tablets, cocaine and LSD.

Métodos probabilístico e determinístico para diagnóstico da necessidade de subsolagem de solos agrícolas

This paper presents two techniques to evaluate soil mechanical resistance to penetration as an auxiliary method to help in a decision-making in subsoiling operations. The decision is based on the volume of soil mobilized as a function of the considered critical soil resistance to penetration in each case. The first method, probabilistic, uses statistical techniques to define the volume of soil to be mobilized. The other method, deterministic, determines the percentage of soil to be mobilized and its spatial distribution. Both cases plot the percentage curves of experimental data related to the soil mechanical resistance to penetration equal or larger to the established critical level and the volume of soil to be mobilized as a function of critical level. The deterministic method plots showed the spatial distribution of the data with resistance to penetration equal or large than the critical level. The comparison between mobilized soil curves as a function of critical level using both methods showed that they can be considered equivalent. The deterministic method has the advantage of showing the spatial distribution of the critical points.

Modelagem matemática e simulação numérica do resfriamento rápido de morango com ar forçado

This work approaches the forced air cooling of strawberry by numerical simulation. The mathematical model that was used describes the process of heat transfer, based on the Fourier's law, in spherical coordinates and simplified to describe the one-dimensional process. For the resolution of the equation expressed for the mathematical model, an algorithm was developed based on the explicit scheme of the numerical method of the finite differences and implemented in the scientific computation program MATLAB 6.1. The validation of the mathematical model was made by the comparison between theoretical and experimental data, where strawberries had been cooled with forced air. The results showed to be possible the determination of the convective heat transfer coefficient by fitting the numerical and experimental data. The methodology of the numerical simulations was showed like a promising tool in the support of the decision to use or to develop equipment in the area of cooling process with forced air of spherical fruits.

Análise de custo-efetividade de métodos preventivos para superfície oclusal de acordo com o risco de cárie: resultados de um ensaio clínico controlado

This study presents the results of a cost-effectiveness analysis in a controlled clinical trial on the effectiveness of a modified glass ionomer resin sealant ( Vitremer, 3M ESPE) and the application of fluoride varnish (Duraphat, Colgate) on occlusal surfaces of first permanent molars in children 6-8 years of age (N = 268), according to caries risk (high versus low). Children were examined semiannually by the same calibrated dentist for 24 months after allocation in six groups: high and low risk controls (oral health education every three months); high and low risk with varnish (oral health education every three months + varnish biannually); and high and low risk with sealant (oral health education every three months + a single application of sealant). Economic analysis showed that sealing permanent first molars of high-risk schoolchildren showed a C/E ratio of US$ 119.80 per saved occlusal surface and an incremental C/E ratio of US$ 108.36 per additional saved occlusal surface. The study concluded that sealing permanent first molars of high-risk schoolchildren was the most cost-effective intervention.

Protocolos de investigação de variáveis psicológicas na epilepsia infantil

Epilepsy is a common chronic condition in the childhood and its diagnosis reveals psychological, social and family difficulties, that seem to be related with beliefs and quality of parents-children interaction. The purpose of this paper is to schematize investigation strategies for the psychological variables: beliefs, impact of the disease, family relationship, identification of changes. Based upon collected reports of epileptic children's parents and upon surveyed aspects of the literature, psychological questionnaires were elaborated to identify important variables that affect the child's epilepsy life and his family. The use of more appropriate investigation procedures facilitates the psychological evaluation and ensures the collection of data.

Estudo comparativo dos métodos de estimativa da idade óssea de Greulich & Pyle e Tanner & Whitehouse

The purpose of this study was to verify whether the Greulich & Pyle (GP), Greulich & Pyle Visual (GPV) and Tanner & Whitehouse (TW) methods for estimating skeletal age could be applied in the Brazilian population, and which of these three methods could be considered more reliable when compared with the chronological age of the individuals. This study was based on one hundred and sixty volunteers (80 females and 80 males) with ages between 6 years and 10 months and 14 years and 9 months. The results showed that for the GP method, the correlations with chronological age were 0.95 for males and 0.97 for females. For the GPV method, the correlations were 0.96 and 0.97, respectively and for TW, 0.96 and 0.97. The results showed that the Greulich & Pyle, Greulich & Pyle Visual and Tanner & Whitehouse methods presented high correlation values when compared with the chronological age of the individuals. Corrective factors were established to make these methods applicable to the Brazilian population.