Sistemas emulsionados para análise de amostras com alto teor lipídico por espectrometria de absorção atômica
Ano de defesa: | 2010 |
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Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | , , , |
Tipo de documento: | Tese |
Tipo de acesso: | Acesso aberto |
Idioma: | por |
Instituição de defesa: |
Universidade Federal de Santa Maria
|
Programa de Pós-Graduação: |
Programa de Pós-Graduação em Química
|
Departamento: |
Química
|
País: |
BR
|
Palavras-chave em Português: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/4193 |
Resumo: | The attention to the knowledge of nutritional and toxicological profiles of foodstuffs is increasing. Therefore, methods that allow for the determination of components desirable or necessary, as essential elements, and of undesirable as heavy metals are of great importance. Atomic Absorption Spectrometry (AAS) is a robust and well established technique for the determination of several elements in the most varied types of samples. Spectrometric analyses are usually made with sample solutions obtained by decomposition processes or sample digestion. However, such procedures result in additional steps that can cause inconveniences such as contamination and losses during manipulation. Emulsified systems have been used in the preparation of samples with high fat content. Emulsifing makes the sample decomposition not necessary, allows reducing the final content of organic matter, and stabilizes the present oily content. In this work, emulsified systems were developed to measure several metals by AAS in samples such as chicken eggs, chocolates, rice oil, canola oil, sunflower oil, corn oil, soy oil, olive oil, margarine light, margarine and butter. The tensoactives used in this work were Triton X100, Triton 114 and Tween 80. Additional oily components, the octila estearato and the corn oil, were used to get better in the stability of the chocolate and egg emulsions. All of the emulsions were prepared using a specific sequence to guarantee the stability and a general procedure of emulsion preparation can be established: to weigh the surfactant, oily sample or additional oily component, when it is the case, and to put in beakers of 80 mL. Adding heated water under continuous agitation to happen the sample emulsification, after following adding water until to reach the final volume. Magnetic agitation should be maintained during the cooling. In the samples of emulsified eggs were determined Selenium (Se) for Graphite Furnace Atomic Absorption Spectrometry (GFAAS) and sodium, potassium, calcium, magnesium, zinc and iron for Flame Atomic Absorption Spectrometry (FAAS). The methods validations were accomplished with the Certified Material of Reference (CRM) Whole Egg Powder (RM 8415). The Se recovery was 95,2% of the certified value and for another metals the recoveries of the certified values varied from 97,5% for magnesium and 102,2% for sodium. The methods showed appropriate sensibility, precision and accuracy. Sodium, potassium, calcium, magnesium, zinc and iron were determined in chocolate samples emulsified by F AAS and micro-emulsions were applied for the determination of aluminum, copper and manganese by GF AAS. The validation of the method was against SRM Baking Chocolate (SRM 2384) and the recoveries of the certified values varied from 88,6% for potassium to 108% for manganses. In the emulsified samples of vegetable oils, margarine and butter were determined As, Cd, Cr, Cu, Mn, Ni and Pb by GF AAS and Na, K, Ca, Mg, Zn and Fe for FAAS. And each in case the best measurement conditions were selected and the operational parameters were fit. The results for accuracy with inorganic recovery assays varied among 90% (Na) to 112% (Fe) for the FAAS measurements and among 83% (Cd) to 121% (Pb) for the GFAAS measurements. |
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2017-05-112017-05-112010-06-04IEGGLI, Carine Viana Silva. Emulsified systems for the analysis of samples with high fat content by atomic absorption spectrometry. 2010. 130 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2010.http://repositorio.ufsm.br/handle/1/4193The attention to the knowledge of nutritional and toxicological profiles of foodstuffs is increasing. Therefore, methods that allow for the determination of components desirable or necessary, as essential elements, and of undesirable as heavy metals are of great importance. Atomic Absorption Spectrometry (AAS) is a robust and well established technique for the determination of several elements in the most varied types of samples. Spectrometric analyses are usually made with sample solutions obtained by decomposition processes or sample digestion. However, such procedures result in additional steps that can cause inconveniences such as contamination and losses during manipulation. Emulsified systems have been used in the preparation of samples with high fat content. Emulsifing makes the sample decomposition not necessary, allows reducing the final content of organic matter, and stabilizes the present oily content. In this work, emulsified systems were developed to measure several metals by AAS in samples such as chicken eggs, chocolates, rice oil, canola oil, sunflower oil, corn oil, soy oil, olive oil, margarine light, margarine and butter. The tensoactives used in this work were Triton X100, Triton 114 and Tween 80. Additional oily components, the octila estearato and the corn oil, were used to get better in the stability of the chocolate and egg emulsions. All of the emulsions were prepared using a specific sequence to guarantee the stability and a general procedure of emulsion preparation can be established: to weigh the surfactant, oily sample or additional oily component, when it is the case, and to put in beakers of 80 mL. Adding heated water under continuous agitation to happen the sample emulsification, after following adding water until to reach the final volume. Magnetic agitation should be maintained during the cooling. In the samples of emulsified eggs were determined Selenium (Se) for Graphite Furnace Atomic Absorption Spectrometry (GFAAS) and sodium, potassium, calcium, magnesium, zinc and iron for Flame Atomic Absorption Spectrometry (FAAS). The methods validations were accomplished with the Certified Material of Reference (CRM) Whole Egg Powder (RM 8415). The Se recovery was 95,2% of the certified value and for another metals the recoveries of the certified values varied from 97,5% for magnesium and 102,2% for sodium. The methods showed appropriate sensibility, precision and accuracy. Sodium, potassium, calcium, magnesium, zinc and iron were determined in chocolate samples emulsified by F AAS and micro-emulsions were applied for the determination of aluminum, copper and manganese by GF AAS. The validation of the method was against SRM Baking Chocolate (SRM 2384) and the recoveries of the certified values varied from 88,6% for potassium to 108% for manganses. In the emulsified samples of vegetable oils, margarine and butter were determined As, Cd, Cr, Cu, Mn, Ni and Pb by GF AAS and Na, K, Ca, Mg, Zn and Fe for FAAS. And each in case the best measurement conditions were selected and the operational parameters were fit. The results for accuracy with inorganic recovery assays varied among 90% (Na) to 112% (Fe) for the FAAS measurements and among 83% (Cd) to 121% (Pb) for the GFAAS measurements.Cresce a atenção para o conhecimento do perfil nutricional e toxicológico dos alimentos. Assim, métodos que permitam a determinação de componentes desejáveis ou necessários, como os elementos essenciais, e de indesejáveis como metais pesados são necessários. A Espectrometria de Absorção Atômica (AAS) é uma técnica robusta e bastante estabelecida para a determinação de vários elementos nos mais variados tipos de amostras. Análises espectrométricas geralmente são feitas em soluções obtidas pelo processo de decomposição ou digestão da amostra original. Entretanto, tais procedimentos implicam em passos adicionais, que podem levar a inconvenientes como contaminação, perdas durante manipulação e a maiores tempos de análise. Sistemas emulsionados têm sido utilizados no preparo de amostras e, como alguns alimentos apresentam alta fração lipídica, esta pode ser uma alternativa conveniente. Com a emulsificação direta com surfactantes não há necessidade de digestão da matéria orgânica e, além disso, permite reduzir o conteúdo final de matéria orgânica e estabilizar o conteúdo oleoso presente. Desenvolveram-se sistemas mulsionados para determinar diversos metais por AAS em amostras de ovos de galinhas, chocolates, óleo de arroz, óleo de canola, óleo de girassol, óleo de milho, óleo de soja, azeite de oliva, margarina light, margarina e manteiga. Os tensoativos utilisaos neste trabalho foram Triton X100, Triton 114 e Tween 80. Componentes oleosos adicionais, o estearato de octila e o óleo de milho, foram utilizados para melhorar a estabilidade das emulsões de ovos e de chocolate. Todas as emulsões foram preparadas usando uma seqüência específica para garantir a sua estabilidade e um procedimento geral de preparo das emulsões pode ser alcançado: as alíquotas de surfactante, amostra oleosa ou componente oleoso, quando for o caso, são pesadas e colocadas em béqueres de 80 mL; água aquecida é adicionada sob agitação contínua, para que ocorra o emulsionamento da amostra, adicionando-se água até completar o volume final. Agitação magnética deve ser mantida durante o arrefecimento. Nas amostras de ovos emulsionados foram determinados de selênio por Espectrometria de Absorção Atômica com Forno de Grafite (GF AAS) e sódio, potássio, cálcio, magnésio, zinco e ferro por Espectrometria de Absorção Atômica com Chama (F AAS). A exatidão dos métodos foi avaliada pela análise do Material de Referência Certificado (MRC) Whole Egg Powder (NIST RM 8415). A recuperação para o Se correspondeu a 95,2% do valor certificado e para os demais metais as recuperações dos valores certificados variaram de 97,5% para magnésio e 102,2% para sódio. Os métodos mostraram adequada sensibilidade, precisão e exatidão. Sódio, potássio, cálcio, magnésio, zinco e ferro foram determinados por F AAS em amostras de chocolate emulsionadas e micro-emulsões foram aplicadas para determinar alumínio, cobre e manganês por GF AAS. Baking Chocolate (SRM 2384) foi utilizado para realizar a validação dos métodos e as recuperações dos valores certificados variaram de 88,6% para potássio a 108% para o manganês. Nas amostras emulsionadas de óleos vegetais, margarina e manteiga, puderam ser determinados As, Cd, Cr, Cu, Mn, Ni e Pb por GF AAS e Na, K, Ca, Mg, Zn e Fe por FAAS. Para cada caso as condições de medida e os parâmetros operacionais foram otimizados. As recuperações variaram entre 90% (Na) a 112% (Fe) para as medidas por F AAS e entre 83% (Cd) a 121% (Pb) para as medidas por GF AAS.Conselho Nacional de Desenvolvimento Científico e Tecnológicoapplication/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em QuímicaUFSMBRQuímicaEmulsõesEspectrometria de absorção atômicaMetaisOvosChocolates e óleos vegetaisEmulsionsAtomic absorption spectrometryMetalsEggsChocolates and edible oilsCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICASistemas emulsionados para análise de amostras com alto teor lipídico por espectrometria de absorção atômicaEmulsified systems for the analysis of samples with high fat content by atomic absorption spectrometryinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisNascimento, Denise Bohrer dohttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4798557Z7Campos, Reinaldo Calixto dehttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4783939H7Vale, Maria Goreti Rodrigueshttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4795696H7Emanuelli, Tatianahttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4797080Z5Rosa, Marcelo Barcellos dahttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4792062P5http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4125303A4Ieggli, Carine Viana Silva1006000000004005003003003005003001c5af0ad-15cf-4a7e-9b25-b8b6b1363ae6fc1680c1-d727-4d4c-b00d-dc0ef7be2d30780e3e34-a078-4d2e-8013-fcdfc4234c3c49d0cf23-7977-4800-92bd-7f73eea8d9797457e618-e257-4f1d-b319-f589826321847ed31110-a771-4a73-9abb-c2a61218cf25info:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALLEGGLI, CARINE VIANA SILVA.pdfapplication/pdf5332904http://repositorio.ufsm.br/bitstream/1/4193/1/LEGGLI%2c%20CARINE%20VIANA%20SILVA.pdf92b911adf112fb3d704984e367a7fffbMD51TEXTLEGGLI, CARINE VIANA SILVA.pdf.txtLEGGLI, CARINE VIANA SILVA.pdf.txtExtracted texttext/plain198962http://repositorio.ufsm.br/bitstream/1/4193/2/LEGGLI%2c%20CARINE%20VIANA%20SILVA.pdf.txt21b0dad4e55e5bc11e4cbe5ae2b59523MD52THUMBNAILLEGGLI, CARINE VIANA SILVA.pdf.jpgLEGGLI, CARINE VIANA SILVA.pdf.jpgIM Thumbnailimage/jpeg5507http://repositorio.ufsm.br/bitstream/1/4193/3/LEGGLI%2c%20CARINE%20VIANA%20SILVA.pdf.jpg0850a84b664bf8da354c90dcf6832c1aMD531/41932022-06-30 12:28:19.142oai:repositorio.ufsm.br:1/4193Repositório Institucionalhttp://repositorio.ufsm.br/PUBhttp://repositorio.ufsm.br/oai/requestopendoar:39132022-06-30T15:28:19Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Sistemas emulsionados para análise de amostras com alto teor lipídico por espectrometria de absorção atômica |
dc.title.alternative.eng.fl_str_mv |
Emulsified systems for the analysis of samples with high fat content by atomic absorption spectrometry |
title |
Sistemas emulsionados para análise de amostras com alto teor lipídico por espectrometria de absorção atômica |
spellingShingle |
Sistemas emulsionados para análise de amostras com alto teor lipídico por espectrometria de absorção atômica Ieggli, Carine Viana Silva Emulsões Espectrometria de absorção atômica Metais Ovos Chocolates e óleos vegetais Emulsions Atomic absorption spectrometry Metals Eggs Chocolates and edible oils CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Sistemas emulsionados para análise de amostras com alto teor lipídico por espectrometria de absorção atômica |
title_full |
Sistemas emulsionados para análise de amostras com alto teor lipídico por espectrometria de absorção atômica |
title_fullStr |
Sistemas emulsionados para análise de amostras com alto teor lipídico por espectrometria de absorção atômica |
title_full_unstemmed |
Sistemas emulsionados para análise de amostras com alto teor lipídico por espectrometria de absorção atômica |
title_sort |
Sistemas emulsionados para análise de amostras com alto teor lipídico por espectrometria de absorção atômica |
author |
Ieggli, Carine Viana Silva |
author_facet |
Ieggli, Carine Viana Silva |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Nascimento, Denise Bohrer do |
dc.contributor.advisor1Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4798557Z7 |
dc.contributor.referee1.fl_str_mv |
Campos, Reinaldo Calixto de |
dc.contributor.referee1Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4783939H7 |
dc.contributor.referee2.fl_str_mv |
Vale, Maria Goreti Rodrigues |
dc.contributor.referee2Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4795696H7 |
dc.contributor.referee3.fl_str_mv |
Emanuelli, Tatiana |
dc.contributor.referee3Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4797080Z5 |
dc.contributor.referee4.fl_str_mv |
Rosa, Marcelo Barcellos da |
dc.contributor.referee4Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4792062P5 |
dc.contributor.authorLattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4125303A4 |
dc.contributor.author.fl_str_mv |
Ieggli, Carine Viana Silva |
contributor_str_mv |
Nascimento, Denise Bohrer do Campos, Reinaldo Calixto de Vale, Maria Goreti Rodrigues Emanuelli, Tatiana Rosa, Marcelo Barcellos da |
dc.subject.por.fl_str_mv |
Emulsões Espectrometria de absorção atômica Metais Ovos Chocolates e óleos vegetais |
topic |
Emulsões Espectrometria de absorção atômica Metais Ovos Chocolates e óleos vegetais Emulsions Atomic absorption spectrometry Metals Eggs Chocolates and edible oils CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Emulsions Atomic absorption spectrometry Metals Eggs Chocolates and edible oils |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
The attention to the knowledge of nutritional and toxicological profiles of foodstuffs is increasing. Therefore, methods that allow for the determination of components desirable or necessary, as essential elements, and of undesirable as heavy metals are of great importance. Atomic Absorption Spectrometry (AAS) is a robust and well established technique for the determination of several elements in the most varied types of samples. Spectrometric analyses are usually made with sample solutions obtained by decomposition processes or sample digestion. However, such procedures result in additional steps that can cause inconveniences such as contamination and losses during manipulation. Emulsified systems have been used in the preparation of samples with high fat content. Emulsifing makes the sample decomposition not necessary, allows reducing the final content of organic matter, and stabilizes the present oily content. In this work, emulsified systems were developed to measure several metals by AAS in samples such as chicken eggs, chocolates, rice oil, canola oil, sunflower oil, corn oil, soy oil, olive oil, margarine light, margarine and butter. The tensoactives used in this work were Triton X100, Triton 114 and Tween 80. Additional oily components, the octila estearato and the corn oil, were used to get better in the stability of the chocolate and egg emulsions. All of the emulsions were prepared using a specific sequence to guarantee the stability and a general procedure of emulsion preparation can be established: to weigh the surfactant, oily sample or additional oily component, when it is the case, and to put in beakers of 80 mL. Adding heated water under continuous agitation to happen the sample emulsification, after following adding water until to reach the final volume. Magnetic agitation should be maintained during the cooling. In the samples of emulsified eggs were determined Selenium (Se) for Graphite Furnace Atomic Absorption Spectrometry (GFAAS) and sodium, potassium, calcium, magnesium, zinc and iron for Flame Atomic Absorption Spectrometry (FAAS). The methods validations were accomplished with the Certified Material of Reference (CRM) Whole Egg Powder (RM 8415). The Se recovery was 95,2% of the certified value and for another metals the recoveries of the certified values varied from 97,5% for magnesium and 102,2% for sodium. The methods showed appropriate sensibility, precision and accuracy. Sodium, potassium, calcium, magnesium, zinc and iron were determined in chocolate samples emulsified by F AAS and micro-emulsions were applied for the determination of aluminum, copper and manganese by GF AAS. The validation of the method was against SRM Baking Chocolate (SRM 2384) and the recoveries of the certified values varied from 88,6% for potassium to 108% for manganses. In the emulsified samples of vegetable oils, margarine and butter were determined As, Cd, Cr, Cu, Mn, Ni and Pb by GF AAS and Na, K, Ca, Mg, Zn and Fe for FAAS. And each in case the best measurement conditions were selected and the operational parameters were fit. The results for accuracy with inorganic recovery assays varied among 90% (Na) to 112% (Fe) for the FAAS measurements and among 83% (Cd) to 121% (Pb) for the GFAAS measurements. |
publishDate |
2010 |
dc.date.issued.fl_str_mv |
2010-06-04 |
dc.date.accessioned.fl_str_mv |
2017-05-11 |
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2017-05-11 |
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info:eu-repo/semantics/publishedVersion |
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info:eu-repo/semantics/doctoralThesis |
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doctoralThesis |
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publishedVersion |
dc.identifier.citation.fl_str_mv |
IEGGLI, Carine Viana Silva. Emulsified systems for the analysis of samples with high fat content by atomic absorption spectrometry. 2010. 130 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2010. |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/4193 |
identifier_str_mv |
IEGGLI, Carine Viana Silva. Emulsified systems for the analysis of samples with high fat content by atomic absorption spectrometry. 2010. 130 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2010. |
url |
http://repositorio.ufsm.br/handle/1/4193 |
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