Submitted by Setor de Tratamento da Informa??o - BC/PUCRS (tede2@pucrs.br) on 2015-05-07T13:39:38Z No. of bitstreams: 1 468073 - Texto Completo.pdf: 2289187 bytes, checksum: e95cc5f55a1d9f82d97c26b1b5b34118 (MD5) / Made available in DSpace on 2015-05-07T13:39:38Z (GMT). No. of bitstreams: 1 468073 - Texto Completo.pdf: 2289187 bytes, checksum: e95cc5f55a1d9f82d97c26b1b5b34118 (MD5) Previous issue date: 2015-01-09 / Carcinogenesis is a complex multifactorial process dependent on inherent to individual or environmental factors. Environmental polycyclic aromatic hydrocarbons (PAHs) have been pointed as a risk factor for different types of cancer, especially in upper aerodigestive tract. Chimarr?o is a hot mat? beverage containing PAHs that are incorporated to the herb during drying process of the leaves. Individuals that drink chimarr?o are exposed do PAHs, which can be assessed by 1-hydroxypyrene-glucuronide levels (1-OHPG). The aim of the present study was to evaluate cytomorphometric alterations of oral mucosa epithelium in chimarr?o drinkers correlating them to salivary and urinary levels of 1-OHPG. Adult males and females without history of regular alcohol use were allocated into 4 groups: (1)=39 chimarr?o drinkers who did not smoke; (2)=25 chimarr?o drinkers who smoked; (3)=27 smokers who did not drink chimarr?o; and (4)=27 individuals who had neither of these habits. Mucosal scrapings were performed and subjected to qualitative (Papanicolaou) and quantitative (nuclear area, cytoplasmic area, nucleus/cytoplasm ratio) analysis. Urine and saliva samples were assayed for 1-OHPG by high-performance liquid chromatography (HPLC). All samples were classified into Papanicolaou class I. Nuclear and cytoplasmic areas of epithelial cells in soft palate smears did not significantly differ between the groups, whereas in buccal (cheek) mucosa they were significantly greater in the chimarr?o group than in controls. The nucleus/cytoplasm ratio as well as salivary and urinary concentrations of 1-OHPG did not significantly differ. Urinary and salivary 1-OHPG concentrations were positively correlated to each other but they did not show any correlation with the cytometric variables. Nuclear and cytoplasmic areas were positively correlated to each other in either palate or buccal mucosa smears. Conclusion : Chimarr?o was associated with neither cytomorphometric alterations in epithelial cells of palate smears nor urinary and salivary 1-OHPG levels. Buccal smears showed higher nuclear and cytoplasmic area in the chimarr?o group, but this result does not support an association with dysplasia. / A carcinog?nese ? um processo complexo e multifatorial dependente de fatores que s?o inerentes ao indiv?duo ou ambientais. A presen?a de hidrocarbonetos arom?ticos polic?clicos (HAPs) no meio ambiente tem sido apontada como um dos fatores de risco para o desenvolvimento de diferentes tipos de c?ncer, principalmente do trato aerodigestivo superior. O chimarr?o ? uma bebida quente ? base de erva-mate que concentra HAPs incorporados ? erva durante o processamento de secagem das folhas. Indiv?duos com o h?bito de tomar chimarr?o est?o expostos aos HAPs, exposi??o esta que pode ser mensurada por meio da quantifica??o de 1-hidroxipireno glucoron?deo (1-OHPG). O presente estudo teve por objetivo investigar altera??es citomorfom?tricas do epit?lio da mucosa oral em tomadores de chimarr?o e correlacion?-las com os n?veis salivares e urin?rios de 1-OHPG. Indiv?duos adultos, de ambos os sexos e sem hist?ria de uso regular de ?lcool, foram distribu?dos em quatro grupos: (1)=39 indiv?duos tomadores de chimarr?o, n?o-fumantes; (2)=25 fumantes tomadores de chimarr?o, (3)=27 indiv?duos fumantes n?o tomadores de chimarr?o e (4)=27 indiv?duos sem nenhum dos h?bitos supracitados (grupo?controle). Amostras de citologia exfoliativa foram obtidas da mucosa do palato mole e mucosa jugal para avalia??o qualitativa (Papanicolaou) e quantitativa (?rea nuclear, ?rea citoplasm?tica e propor??o n?cleo/citoplasma). Amostras de saliva e urina foram coletadas para dosagem de 1-OHPG por meio de cromatografia l?quida de alta performance (HPLC). Os resultados evidenciaram todas as amostras citol?gicas classificadas como classe I de Papanicolaou. As ?reas nuclear e citoplasm?tica das c?lulas epiteliais do palato, bem como a propor??o n?cleo/citoplasma de ambos os s?tios n?o diferiram significativamente entre os grupos. No grupo chimarr?o, as c?lulas epiteliais da mucosa jugal exibiram ?rea nuclear e ?rea citoplasm?tica significativamente maiores que o grupo-controle. Foi observada correla??o positiva entre ?rea nuclear e citoplasm?tica, bem como entre concentra??es salivares e urin?rias de 1-OHPG. Conclus?o : N?o foi observada associa??o do chimarr?o com altera??es citomorfom?tricas das c?lulas epiteliais do palato, ou com os n?veis salivares e urin?rios de 1-OHPG. Embora ?rea nuclear e citoplasm?tica tenham sido significativamente maiores no grupo chimarr?o do que no controle, o presente estudo n?o permite inferir que essas altera??es tenham tend?ncia displ?sica.

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2017-03-09T19:05:35Z No. of bitstreams: 1 TeresaCristinaEpifanioDiogenesRego_TESE.pdf: 2814198 bytes, checksum: b7ac8c1062e9b9486287153d37e0b630 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2017-03-10T21:49:04Z (GMT) No. of bitstreams: 1 TeresaCristinaEpifanioDiogenesRego_TESE.pdf: 2814198 bytes, checksum: b7ac8c1062e9b9486287153d37e0b630 (MD5) / Made available in DSpace on 2017-03-10T21:49:04Z (GMT). No. of bitstreams: 1 TeresaCristinaEpifanioDiogenesRego_TESE.pdf: 2814198 bytes, checksum: b7ac8c1062e9b9486287153d37e0b630 (MD5) Previous issue date: 2015-07-24 / A utiliza??o de agrot?xicos da classe dos organofosforados e dos carbamatos a partir das d?cadas de 1940 e 1950 no Brasil trouxe benef?cios no combate as pragas em lavouras de alimentos mas tamb?m causou impactos negativos ? sa?de humana e ao meio ambiente, devido ? presen?a desses compostos nos alimentos, na ?gua e no solo. Diante disso, torna-se essencial o desenvolvimento de m?todos anal?ticos para determina??o multirres?duos de agrot?xicos em matrizes ambientais e de alimentos. Neste trabalho otimizou-se e validou-se uma metodologia anal?tica para a determina??o de agrot?xicos da classe dos carbamatos (carbaril e carbofurano), organofosforados (clorpirif?s, dimetoato, malationa e metamidof?s) e do neonicotin?ide acetamiprido em amostras de alface e solo, utilizando QuEChERS e Cromatografia L?quida de fase reversa acoplada ? espectrometria de massas com ioniza??o por Electrospray (LC-ESI/MS/MS), operada em modo de Monitoramento de Rea??es M?ltiplas (MRM). O m?todo de preparo de amostra QuEChERS originalmente desenvolvido para an?lise de alimentos, neste trabalho foi otimizado tanto na an?lise de amostras de alface, como tamb?m em amostras de solo, buscando-se um m?todo r?pido, pr?tico e eficiente de preparo de amostras ambientais. Para atender aos objetivos propostos, foram feitas adi??es dos sete agrot?xicos ao n?vel de fortifica??o de 5,0 ?g kg-1 em amostras de alface e solo, obtendo recupera??es entre 67,8-102,7% em alface, e entre 73-121,1% em solo, com repetibilidade e precis?o intermedi?ria com coeficientes de varia??o inferior a 15% para ambas as matrizes e limite de quantifica??o de 1,0 ?g kg-1 para os sete agrot?xicos. O efeito matriz nas amostras selecionadas foi contornado diluindo-se os extratos. Para verificar a aplicabilidade do m?todo otimizado e validado foram coletadas amostras de alface e solo diretamente dos produtores da regi?o de Gramorezinho, localizada na Zona Norte de Natal/RN, onde nenhum dos sete padr?es de agrot?xicos pesquisados foi encontrado; como este estudo foi realizado numa comunidade de produtores de hortali?as em que o cultivo convencional com agrot?xicos, foi convertido em produ??o org?nica, o fato da n?o quantifica??o dos compostos estudados confirma a descontinuidade do uso destas subst?ncias pelos agricultores selecionados. / The use of pesticides in the class of organophosphates and carbamates from the 1940s and 1950s in Brazil brought benefits in combating pests on food crops, but also caused negative impacts to human health and the environment due to the presence of these compounds in food, water and soil. Therefore, it is essential to develop analytical methods for Multiresidue determination of pesticides in food and environmental matrices. This work is optimized and validated an analytical methodology for the determination of pesticides in the class of carbamates (carbaryl and carbofuran), organophosphates (chlorpyrifos, dimethoate, malathion and methamidophos) and neonicotinoid acetamiprid in samples of lettuce and ground using QuEChERS and reverse-phase liquid chromatography coupled to mass spectrometry with electrospray ionization (ESI-LC/MS/MS) operated in Mode Reaction Monitoring Multiple (MRM); the sample preparation QuEChERS method originally developed for food analysis, this work has been optimized both in the analysis of samples of lettuce, as well as in soil samples, seeking a fast, practical and efficient preparation of environmental samples. To meet the proposed objectives, additions of the seven pesticides at the level of fortification 5.0 ?g kg-1 in samples of lettuce and soil were made, obtaining recoveries between 67.8 to 102.7% in lettuce, and between 73-121.1% in soil, with repeatability and intermediate precision with coefficients of variation below 15% for both matrices and quantitation limit of 1.0 ?g kg-1 for seven pesticides; the effect matrix in selected samples was circumvented by diluting the extracts. To verify the applicability of the optimized and validated method were collected samples of lettuce and soil directly from producers, none of the seven pesticides standards researched found; as this study was conducted in a vegetable producing community than conventional cultivation, or with pesticides, it has been converted to organic production, the fact that no quantification of the compounds studied confirms the discontinuance of the use of these substances by selected farmers.

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2017-11-01T21:32:49Z No. of bitstreams: 1 KarinaCavalcanteDeOliveira_DISSERT.pdf: 1728605 bytes, checksum: 96c5810c528f87422422321c78049b6c (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2017-11-08T00:03:54Z (GMT) No. of bitstreams: 1 KarinaCavalcanteDeOliveira_DISSERT.pdf: 1728605 bytes, checksum: 96c5810c528f87422422321c78049b6c (MD5) / Made available in DSpace on 2017-11-08T00:03:54Z (GMT). No. of bitstreams: 1 KarinaCavalcanteDeOliveira_DISSERT.pdf: 1728605 bytes, checksum: 96c5810c528f87422422321c78049b6c (MD5) Previous issue date: 2017-02-02 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior (CAPES) / O uso de agrot?xicos t?m trazido enormes benef?cios em termos de aumento da produ??o e qualidade dos produtos agr?colas. Contudo, o uso indiscriminado dos agrot?xicos representa um risco para sa?de humana, sendo a ingest?o de alimentos uma das principais formas de exposi??o a essas subst?ncias t?xicas. Neste trabalho, foi desenvolvido e validado um m?todo anal?tico para determina??o multiresidual de 10 carbamatos (aldicarbe, aldicarbe sulf?xido, aldicarbe sulfona, carbaril, carbofurano, 3-hidroxicarbofurano, metiocarbe, metomil, oxamyl e propoxur) em piment?es comercializados na cidade de Natal/ RN. O desenvolvimento do m?todo consistiu na extra??o em fase s?lida manual seguida de an?lise por Cromatografia L?quida de Alta Efici?ncia acoplada com detector de arranjo de fotodiodos para a regi?o do UV-Vis?vel. Na valida??o foi avaliada a sensibilidade, linearidade, precis?o, exatid?o, limite de detec??o, limite de quantifica??o e robustez. As curvas anal?ticas apresentaram linearidade entre 0,1 e 1,1 mg L-1 para o aldicarbe sulfona, propoxur, carbaril e 3-hidroxicarbofurano, entre 0,1 e 0,9 mg L-1 para o carbofurano e entre 0,3 e 1,1 mg L-1 para o aldicarbe sulf?xido, oxamyl, metomil, aldicarbe e metiocarbe. Os coeficientes de correla??o variaram entre 0,9599 e 0,9939. O limite de detec??o (LD) ficou entre 0,0216 e 0,1319 mg L-1 e o limite de quantifica??o (LQ) entre 0,0719 e 0,4395. O m?todo tamb?m apresentou boa precis?o, com todos os valores de desvio padr?o relativos inferiores a 20%. A extra??o que apresentou melhor resultado foi a que n?o continha carv?o ativado, mas tinha a presen?a do tamp?o de ?cido ac?tico. Foi poss?vel recuperar o aldicarbe sulf?xido, 74,8%, oxamyl, 110,0%, metomil, 150,0%, e aldicarbe, 55,0%. / The use of agrochemicals have brought enormous benefits in terms of increasing production and quality of agricultural products. However, the indiscriminate use of agrochemicals represents a risk to human health, being the food intake one of the main forms of exposure to these toxic substances. An analytical method for the determination of 10 carbamates (aldicarb, aldicarb sulfoxide, aldicarb sulfone, carbaryl, carbofuran, 3-hydroxycarbbofuran, methiocarb, methomyl, oxamyl and propoxur) was developed and validated in green chillies sold in the city of Natal / RN. The development of the method consisted of manual Solid Phase Extraction followed by High Performance Liquid Chromatography coupled with photodiode arrangement detector for the UV-Visible region. In the validation the sensitivity, linearity, precision, accuracy, detection limit, quantification limit and robustness were evaluated. The analytical curves showed linearity between 0.1 and 1.1 mg L-1 for aldicarb sulfone, propoxur, carbaryl and 3-hydroxycarbofuran, between 0.1 and 0.9 mg L-1 for carbofuran and between 0.3 and 1.1 mg L-1 for the aldicarb sulfoxide, oxamyl, methomyl, aldicarb and methiocarb. The correlation coefficients ranged from 0.9599 to 0.9939. The detection limit (DL) was between 0.0216 and 0.1319 mg L-1 and the quantification limit (LQ) was between 0.0719 and 0.4395. The method also showed good accuracy, with all relative standard deviation values lower than 20%. The extraction that presented the best result was the one that did not contain activated carbon, but had the presence of the acetic acid buffer. It was possible to recover aldicarb sulfoxide, 74.8%, oxamyl, 110.0%, methomyl, 151.0%, and aldicarb, 55.0%

Made available in DSpace on 2014-12-17T14:16:30Z (GMT). No. of bitstreams: 1 MarceloVPA_DISSERT.pdf: 3152615 bytes, checksum: 2a3513c0df769468fec98423bf2dba29 (MD5) Previous issue date: 2013-03-21 / Tuberculosis is a serious disease, but curable in practically 100% of new cases, since complied the principles of modern chemotherapy. Isoniazid (ISN), Rifampicin (RIF), Pyrazinamide (PYR) and Chloride Ethambutol (ETA) are considered first line drugs in the treatment of tuberculosis, by combining the highest level of efficiency with acceptable degree of toxicity. Concerning USP 33 - NF28 (2010) the chromatography analysis to 3 of 4 drugs (ISN, PYR and RIF) last in average 15 minutes and 10 minutes more to obtain the 4th drug (ETA) using a column and mobile phase mixture different, becoming its industrial application unfavorable. Thus, many studies have being carried out to minimize this problem. An alternative would use the UFLC, which is based with the same principles of HPLC, however it uses stationary phases with particles smaller than 2 ?m. Therefore, this study goals to develop and validate new analytical methods to determine simultaneously the drugs by HPLC/DAD and UFLC/DAD. For this, a analytical screening was carried out, which verified that is necessary a gradient of mobile phase system A (acetate buffer:methanol 94:6 v/v) and B (acetate buffer:acetonitrile 55:45 v/v). Furthermore, to the development and optimization of the method in HPLC and UFLC, with achievement of the values of system suitability into the criteria limits required for both techniques, the validations have began. Standard solutions and tablets test solutions were prepared and injected into HPLC and UFLC, containing 0.008 mg/mL ISN, 0.043 mg/mL PYR, 0.030 mg.mL-1 ETA and 0.016 mg/mL RIF. The validation of analytical methods for HPLC and UFLC was carried out with the determination of specificity/selectivity, analytical curve, linearity, precision, limits of detection and quantification, accuracy and robustness. The methods were adequate for determination of 4 drugs separately without interfered with the others. Precise, due to the fact of the methods demonstrated since with the days variation, besides the repeatability, the values were into the level required by the regular agency. Linear (R> 0,99), once the methods were capable to demonstrate results directly proportional to the concentration of the analyte sample, within of specified range. Accurate, once the methods were capable to present values of variation coefficient and recovery percentage into the required limits (98 to 102%). The methods showed LOD and LOQ very low showing the high sensitivity of the methods for the four drugs. The robustness of the methods were evaluate, facing the temperature and flow changes, where they showed robustness just with the preview conditions established of temperature and flow, abrupt changes may influence with the results of methods / A tuberculose ? uma doen?a grave, por?m cur?vel em praticamente 100% dos casos novos, desde que obedecidos os princ?pios da moderna quimioterapia. S?o considerados f?rmacos de 1? linha no tratamento ? tuberculose: isoniazida, pirazinamida, etambutol e rifampicina. De acordo com USP 33 - NF28 (2010) as an?lises cromatogr?ficas para 3 dos 4 f?rmacos (isoniazida, pirazinamida e rifampicina) duram em m?dia 15 minutos e mais 10 minutos para a obten??o do 4? f?rmaco (etambutol) utilizando outra coluna, com outra mistura de fase m?vel, tornando esta aplica??o na pr?tica industrial desfavor?vel. Uma das alternativas ? utilizar o CLUE, o qual baseia-se nos mesmos princ?pios da CLAE, por?m utiliza fases estacion?rias com part?culas menores que 2 ?m. Dessa forma pretende-se com o presente estudo desenvolver e validar novos m?todos anal?ticos para determina??o simult?nea de tuberculost?ticos por CLAE/DAD e CLUE/DAD. Para isto, foi realizado um screening anal?tico, o qual verificou que ? necess?rio um gradiente de sistema de fase m?vel A (tamp?o acetato:metanol 94:6 v/v) e B (tamp?o acetato:acetonitrila 55:45 v/v). Posteriormente, ao desenvolvimento e otimiza??o do m?todo em CLAE e CLUE com a obten??o dos valores de adequabilidade do sistema dentro dos limites de aceita??es vigente para ambos as t?cnicas, as valida??es deram-se in?cio. Solu??es padr?es e solu??es testes dos comprimidos foram preparadas e injetadas no CLAE e CLUE, contendo isoniazida, pirazinamida, etambutol e rifampicina nas concentra??es de 0,008, 0,043, 0,030 e 0,016 mg.mL-1, respectivamente. A valida??o dos m?todos anal?ticos foram realizadas para: especificidade / seletividade, intervalos da curva anal?tica, linearidade, limite de detec??o, limite de quantifica??o, exatid?o, precis?o (repetibilidade, precis?o intermedi?ria) e robustez. Os m?todos foram adequados para determina??o dos 4 f?rmacos separadamente sem interfer?ncia nos demais. Precisos, devido ao fato de que os m?todos demonstraram que mesmo com varia??o de dias, al?m da repetibilidade, os valores ficaram dentro da faixa preconizada na legisla??o vigente. Lineares (R > 0,99), ou seja, os m?todos foram capazes de demonstrar que os resultados obtidos eram diretamente proporcionais ? concentra??o do analito na amostra, dentro de um intervalo especificado. Exatos, uma vez que os m?todos foram capazes de apresentar valores de coeficiente de varia??o e porcentagem de recupera??o dentro dos limites exigidos (98 a 102%). Os m?todos mostraram LD e LQ com n?veis baixos demonstrando que os m?todos possuem elevada sensibilidade aos quarto f?rmacos. A robustez foi avaliada frente ?s altera??es de temperatura e fluxo, onde os m?todos demonstraram-se robustos apenas nas condi??es previamente estabelecidas de temperatura e fluxo, altera??es bruscas podem acarretar influ?ncia nos resultados dos m?todos

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2016-07-06T19:31:44Z No. of bitstreams: 1 AlessandraMirandaCabral_TESE.pdf: 6365210 bytes, checksum: 82d82db05530ac0319ed9de4c089f191 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2016-07-06T21:16:55Z (GMT) No. of bitstreams: 1 AlessandraMirandaCabral_TESE.pdf: 6365210 bytes, checksum: 82d82db05530ac0319ed9de4c089f191 (MD5) / Made available in DSpace on 2016-07-06T21:16:55Z (GMT). No. of bitstreams: 1 AlessandraMirandaCabral_TESE.pdf: 6365210 bytes, checksum: 82d82db05530ac0319ed9de4c089f191 (MD5) Previous issue date: 2015-12-18 / A Benzilpenicilina (PENG) ? usada como princ?pio ativo em medicamentos veterin?rios, para aumentara produtividade pecu?ria, devido suas propriedades terap?uticas. Este antibi?tico ? indicado para controle de infec??es em animais produtores de alimentos, como bovinos e caprinos. Por?m, quando s?o de m? qualidade e utilizados indiscriminadamente, resultam em res?duos nos alimentos expostos ao consumo humano, principalmente, no leite que ? essencial para dieta das popula??es de crian?as e idosos. Assim, ? imprescind?vel que se desenvolvam novos m?todos capazes de detectar os res?duos nesse alimento, em n?veis que s?o nefastos a sa?de humana, a fim de contribuir com a seguran?a alimentar dos consumidores e colaborar com as ag?ncias reguladoras numa fiscaliza??o eficiente. Este trabalho oferece um novo m?todo, para determina??ode res?duos dos antibi?ticos. Aqui, mostramos duas etapas para controle anal?tico, na primeira ? constatado, pelas medidas das propriedades f?sico-qu?micas, a identidade e qualidade desses f?rmacos, comercialmente distribu?dos. Na segunda etapa, foi desenvolvido e validado um novo m?todo para extra??o, identifica??o e quantifica??o de PENG utilizando Cromatografia liquida ultra-r?pida acoplada a arranjo linear de fotodiodos (UFLC-DAD). Este m?todo foi aplicado em amostras de leite ultrapasterizado bovino (m?todo 1) e caprino (m?todo 2). O m?todo 1 apresentou limite de detec??o (LD) 7,246 ? 10-4?g mL-1. Limite de quantifica??o (LQ) 2,196 ? 10-3?g mL-1. O m?todo 2 apresentou LD de 8,251 ? 10-4 ?g mL-1. LQ de 2,5270 ? 10-3 ?g mL-1. Os resultados mostraram concord?ncia com o limite m?ximo de res?duos (LMR)de 4 ? 10-3 ?g mL-1em 88% para leite bovino e 85% para leite caprino. Os m?todos desenvolvidos se apresentam como uma excelente ferramenta a ser utilizada na investiga??o dos res?duos de antibi?ticos em leite. Sobretudo porque os procedimentos desenvolvidos apresentaram simplicidade, seletividade, reduzido tempo de an?lise e consumo de reagentes e solventes t?xicos, se comparados ?s metodologias j? estabelecidas. / 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 ? 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 ?g mL-1. LOQ of 2.049 ? 10-3 ?g 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 ?g Kg-1 standardized by CAC/GL16. Validation of the method 1 indicated R by 0.9975. LOD of 7.246 ? 10-4 ?g mL-1. LOQ de 2.196 ? 10-3 ?g 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 ?g mL-1. LOQ de 2.5270 ? 10-3 ?g 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.

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2017-02-13T19:44:49Z No. of bitstreams: 1 GrazieneLopesDeSouza_DISSERT.pdf: 1409638 bytes, checksum: b2258a2f626dcdfadfc00445de366ca7 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2017-02-14T21:07:25Z (GMT) No. of bitstreams: 1 GrazieneLopesDeSouza_DISSERT.pdf: 1409638 bytes, checksum: b2258a2f626dcdfadfc00445de366ca7 (MD5) / Made available in DSpace on 2017-02-14T21:07:26Z (GMT). No. of bitstreams: 1 GrazieneLopesDeSouza_DISSERT.pdf: 1409638 bytes, checksum: b2258a2f626dcdfadfc00445de366ca7 (MD5) Previous issue date: 2015-06-26 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior (CAPES) / Anacardium occidentale Linn ? uma ?rvore nativa do Brasil, popularmente conhecida como cajueiro. Estudos mostram que a fra??o Acetato de Etila (AcOEt) obtida a partir do extrato acetona das cascas do caule de A. occidentale apresenta atividade anti-inflamat?ria, sugerindo-se os taninos como respons?veis por essa a??o. Sendo uma das 71 esp?cies da Rela??o Nacional de Plantas Medicinais de Interesse ao Sistema ?nico de Sa?de (RENISUS), ? importante que sejam desenvolvidas metodologias anal?ticas para o estudo dos seus constituintes. Nesse contexto, a Cromatografia L?quida de Alta Efici?ncia (CLAE) constitui uma metodologia de import?ncia para a an?lise de amostras de origem vegetal. Este estudo teve como objetivo desenvolver e validar uma metodologia anal?tica por CLAE para a an?lise da fra??o AcOEt do extrato acetona das cascas do caule de A. occidentale. As condi??es cromatogr?ficas foram estabelecidas utilizando como fase m?vel ?cido ac?tico a 0,3% e acetonitrila. Como ponto de partida para o desenvolvimento do m?todo cromatogr?fico, foi utilizado um gradiente explorat?rio, que permite analisar todas as faixas de polaridade. O gradiente de elui??o foi ent?o ajustado at? a obten??o de um cromatograma com adequada separa??o e par?metros cromatogr?ficos satisfat?rios. Para a identifica??o dos compostos, foi realizada a an?lise de padr?es e, pela observa??o dos tempos de reten??o e espectros de absor??o das subst?ncias, foi poss?vel eleger as que estariam presentes na amostra. Foi poss?vel sugerir a presen?a de catequina, epicatequina, epigalocatequina e ?cido g?lico na fra??o AcOEt de A. occidentale. Para a valida??o do m?todo, foram realizados os testes de linearidade, precis?o, exatid?o, robustez, limites de detec??o e quantifica??o. O m?todo foi avaliado como sendo linear, preciso e exato para os compostos estudados. Dentre as condi??es de an?lise alteradas para o estudo da robustez, o m?todo n?o apresentou robustez para a an?lise do ?cido g?lico, quando a temperatura da coluna foi de 35?C, mas as demais condi??es alteradas n?o promoveram mudan?as estatisticamente significativas para este analito. Conclui-se que o m?todo cromatogr?fico ? adequado para a an?lise da fra??o AcOEt do extrato acetona de A. occidentale. / Anacardium occidentale Linn is a tree native to Brazil, popularly known as cashew. Studies show that the Ethyl Acetate fraction (EtOAc) obtained from the acetone:water extract of the A. occidentale stem bark has anti-inflammatory activity, suggesting tannins as responsible for this action. As one of 71 species of the National List of Medicinal Plants of Interest to the Unified Health System (RENISUS), it is important that analytical methodologies for the study of its constituents are developed. In this context, the High Performance Liquid Chromatography (HPLC) is a method of importance to the analysis of samples of plant origin. This study aimed to develop and validate an analytical methodology by HPLC for analysis of EtOAc fraction of acetone:water extract from the stem bark of A. occidentale. The chromatographic conditions were established using acetic acid 0.3% (v/v in water) and acetonitrile as the mobile phase. As a starting point for the development of chromatographic procedures, exploratory gradient was used, which allows to analyze all polarity groups. The gradient elution was then adjusted to obtain a chromatogram with adequate separation and satisfactory chromatographic parameters. For identification of the compounds, the pattern analysis was carried out, and by observing the retention times and absorption spectra of the substances was possible to choose those which would be present in the sample. It could suggest the presence of catechin, epicatechin, epigallocatechin and gallic acid in the EtOAc fraction of A. occidentale. To validate the method, linearity tests were performed, precision, accuracy, robustness, limits of detection and quantification. According to Resolution 899/2003 (ANVISA), the method was assessed to be linear, precise and accurate for the studied compounds. Among the changed analysis conditions for studying the robustness of the method, when the column temperature was 35?C analysis did not present robustness for gallic acid, but when other conditions were changed it did not promote statistically significant changes to this analyte. It follows that the chromatographic method is suitable for analysis of gallic acid, catechin and epicatechin in EtOAc fraction of the acetone:water extract of the A. occidentale.