Espectroscopia Raman amplificada por superfície associada à cromatografia em camada delgada para análise de amostras alimentícias
Ano de defesa: | 2018 |
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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 São Carlos
Câmpus São Carlos |
Programa de Pós-Graduação: |
Programa de Pós-Graduação em Química - PPGQ
|
Departamento: |
Não Informado pela instituição
|
País: |
Não Informado pela instituição
|
Palavras-chave em Português: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | https://repositorio.ufscar.br/handle/ufscar/10272 |
Resumo: | Surface enhancement Raman spectroscopy (SERS) presents the advantages of conventional Raman spectroscopy with the possibility to detect compounds in low levels due to the enhancement on Raman intensity, generated by the molecule-nanoparticle system. Thin-layer chromatography (TLC) is a fast and easy separation technique, that can be coupled to several analytical techniques in order to identify compounds. TLC-SERS is a relatively new technique, with only a few works published; however it presents the advantages of both techniques synergically. The use of nanoparticles adsorbed onto the TLC plate enables to obtain Raman spectra of the separated compounds even in low concentrations. Therefore, this work proposes the use of TLC-SERS in three different application of food interest: product authentication, food safety and stability studies. 1) In product authentication, it was analyzed Pilsner beer samples in order to obtain pattern recognition related to brand and brewery. Samples were prepared in TLC plates and sprayed with gold nanoparticle to promote SERS analysis regarding the elution line of the target analytes. The obtained results were compared by two chemometric methods of data decomposition and signal recovering: multivariate curve resolution (MCR) and independent component analysis (ICA). From the obtained chromatographic peaks was possible to perform fingerprint analysis and identify clustering pattern concerning sample brand and brewery location. 2) As food safety application, the aim was to develop and optimize an analytical methodology to quantify two veterinary drugs (sulfamethoxazole and trimethoprim) in bovine milk. Central composite design was applied evaluating NaCl concentration and nanoparticles pre-concentration to optimize the analytical signal. The hyperspectral images obtained from TLC-SERS were processed using different chemometric methods. For trimethoprim, it was obtained recoveries of 82 – 112% in milk samples. Due to the high complexity of the samples, it was not possible to obtain reliable quantitative values for sulfamethoxazole. 3) For the stability study, it was kinetically assessed one red wine sample under different degradation conditions. For this, it was used a 2³ design of experiments varying pH, dissolved O2 and the presence of anti-oxidant agent. Samples were left in three stocking temperatures (4, 24 and 40 °C) and evaluated during 45 days. SERS chromatograms were analyzed using ICA, and from the chromatographic profile, it was possible to perform ANOVA-PCA where it was identified temperature and the presence of anti-oxidant agent as the most significant variables. |
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Soares, Frederico Luis FelipeCarneiro, Renato Lajarimhttp://lattes.cnpq.br/8065852319463976http://lattes.cnpq.br/10646208471071892018-07-11T11:51:02Z2018-07-11T11:51:02Z2018-04-13SOARES, Frederico Luis Felipe. Espectroscopia Raman amplificada por superfície associada à cromatografia em camada delgada para análise de amostras alimentícias. 2018. Tese (Doutorado em Química) – Universidade Federal de São Carlos, São Carlos, 2018. Disponível em: https://repositorio.ufscar.br/handle/ufscar/10272.https://repositorio.ufscar.br/handle/ufscar/10272Surface enhancement Raman spectroscopy (SERS) presents the advantages of conventional Raman spectroscopy with the possibility to detect compounds in low levels due to the enhancement on Raman intensity, generated by the molecule-nanoparticle system. Thin-layer chromatography (TLC) is a fast and easy separation technique, that can be coupled to several analytical techniques in order to identify compounds. TLC-SERS is a relatively new technique, with only a few works published; however it presents the advantages of both techniques synergically. The use of nanoparticles adsorbed onto the TLC plate enables to obtain Raman spectra of the separated compounds even in low concentrations. Therefore, this work proposes the use of TLC-SERS in three different application of food interest: product authentication, food safety and stability studies. 1) In product authentication, it was analyzed Pilsner beer samples in order to obtain pattern recognition related to brand and brewery. Samples were prepared in TLC plates and sprayed with gold nanoparticle to promote SERS analysis regarding the elution line of the target analytes. The obtained results were compared by two chemometric methods of data decomposition and signal recovering: multivariate curve resolution (MCR) and independent component analysis (ICA). From the obtained chromatographic peaks was possible to perform fingerprint analysis and identify clustering pattern concerning sample brand and brewery location. 2) As food safety application, the aim was to develop and optimize an analytical methodology to quantify two veterinary drugs (sulfamethoxazole and trimethoprim) in bovine milk. Central composite design was applied evaluating NaCl concentration and nanoparticles pre-concentration to optimize the analytical signal. The hyperspectral images obtained from TLC-SERS were processed using different chemometric methods. For trimethoprim, it was obtained recoveries of 82 – 112% in milk samples. Due to the high complexity of the samples, it was not possible to obtain reliable quantitative values for sulfamethoxazole. 3) For the stability study, it was kinetically assessed one red wine sample under different degradation conditions. For this, it was used a 2³ design of experiments varying pH, dissolved O2 and the presence of anti-oxidant agent. Samples were left in three stocking temperatures (4, 24 and 40 °C) and evaluated during 45 days. SERS chromatograms were analyzed using ICA, and from the chromatographic profile, it was possible to perform ANOVA-PCA where it was identified temperature and the presence of anti-oxidant agent as the most significant variables.A espectroscopia Raman amplificada por superfície (SERS), apresenta as vantagens da espectroscopia Raman convencional com a possibilidade de detectar compostos em menores concentrações devido ao aumento na intensidade Raman gerada pelo sistema molécula-nanopartícula. A cromatografia de camada delgada (CCD) é uma técnica de separação rápida, fácil e que pode ser associada a diversas técnicas analíticas com o intuito de identificar e detectar os compostos separados. A SERS-CCD é uma técnica pouco estudada, mas que apresenta as vantagens de ambas as técnicas de maneira sinérgica. A utilização de nanopartículas adsorvidas nas placas de CCD reveladas possibilita adquirir espectros Raman dos compostos separados mesmo em baixas concentrações. Neste trabalho, propõe-se a utilização da SERS-CCD em três diferentes aplicações de interesse alimentar: autenticação de produto, segurança alimentar e estudo de estabilidade. 1) Na autenticação de produto, foram analisadas amostras de cerveja Pilsner com o intuito de se obter padrões de agrupamentos relativos a marca e local de produção. As amostras foram separadas em placas de CCD e borrifadas pela solução coloidal de nanopartículas de ouro para análises SERS ao longo da linha de separação. Comparou-se dois métodos quimiométricos de decomposição de dados e recuperação de sinais, a resolução de curvas multivariadas (MCR) e análise por componentes independentes (ICA). A partir dos picos cromatográficos obtidos, pôde-se realizar uma análise de fingerprint das amostras e identificou-se padrões de agrupamento a partir da marca e local de fabricação. 2) Como aplicação em segurança alimentar, teve-se como objetivo desenvolver e otimizar uma método analítica para a quantificação de dois fármacos de uso veterinário (sulfametoxazol e trimetoprima) em amostras de leite. Um planejamento composto central foi aplicado investigando a concentração de NaCl nas nanopartículas e a pré-concentração das mesmas para otimizar o sinal analítico. As imagens hiperspectrais geradas a partir da análise por SERS-CCD foram tratadas com diferentes métodos quimiométricos. Para trimetoprima foi obtido recuperações de 82 a 118%. Devido à complexidade da amostra, não foi possível obter valores quantitativos confiáveis para sulfametoxazol. 3) Para o estudo de estabilidade, avaliou-se cineticamente uma amostra de vinho tinto submetida a diferentes condições de degradação. Para isso, utilizou-se um planejamento experimental de 2³ com as variáveis pH da solução, quantidade de O2 dissolvido e a presença de agente antioxidante. As amostras foram submetidas a três temperaturas de estocagem (4, 24 e 40 °C) e avaliadas durante 45 dias. Os cromatogramas SERS foram analisados utilizando ICA, e a partir dos picos cromatográficos obtidos, pôde-se realizar uma ANOVA-PCA onde identificou-se as variáveis temperatura e agente antioxidante como as mais significativas para a alteração da amostra.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)porUniversidade Federal de São CarlosCâmpus São CarlosPrograma de Pós-Graduação em Química - PPGQUFSCarQuimiometriaCervejaLeiteVinhoSERSTLCChemometricsBeerMilkWineCIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICAEspectroscopia Raman amplificada por superfície associada à cromatografia em camada delgada para análise de amostras alimentíciasSurface enhancement Raman spectroscopy coupled to thin-layer chromatography for analysis of food samplesDiffusion Raman exaltée par effet de surface associée à chromatographie sur couche mince pour l'analyse d'échantillons alimentairesinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisOnlineinfo:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFSCARinstname:Universidade Federal de São Carlos (UFSCAR)instacron:UFSCARORIGINALTese_FLFS.pdfTese_FLFS.pdfapplication/pdf7357194https://{{ getenv "DSPACE_HOST" "repositorio.ufscar.br" }}/bitstream/ufscar/10272/1/Tese_FLFS.pdf9e987753e58d126d0ee6e2812cd8ff76MD51LICENSElicense.txtlicense.txttext/plain; charset=utf-81957https://{{ getenv "DSPACE_HOST" "repositorio.ufscar.br" }}/bitstream/ufscar/10272/4/license.txtae0398b6f8b235e40ad82cba6c50031dMD54TEXTTese_FLFS.pdf.txtTese_FLFS.pdf.txtExtracted texttext/plain268014https://{{ getenv "DSPACE_HOST" "repositorio.ufscar.br" }}/bitstream/ufscar/10272/5/Tese_FLFS.pdf.txt414cdfcfc5dae18b46e64210dd44e6ffMD55THUMBNAILTese_FLFS.pdf.jpgTese_FLFS.pdf.jpgIM Thumbnailimage/jpeg9437https://{{ getenv "DSPACE_HOST" "repositorio.ufscar.br" }}/bitstream/ufscar/10272/6/Tese_FLFS.pdf.jpge00eb0de07351f97d734f3569616e5cdMD56ufscar/102722019-09-11 03:18:11.603oai:repositorio.ufscar.br:ufscar/10272TElDRU7Dh0EgREUgRElTVFJJQlVJw4fDg08gTsODTy1FWENMVVNJVkEKCkNvbSBhIGFwcmVzZW50YcOnw6NvIGRlc3RhIGxpY2Vuw6dhLCB2b2PDqiAobyBhdXRvciAoZXMpIG91IG8gdGl0dWxhciBkb3MgZGlyZWl0b3MgZGUgYXV0b3IpIGNvbmNlZGUgw6AgVW5pdmVyc2lkYWRlCkZlZGVyYWwgZGUgU8OjbyBDYXJsb3MgbyBkaXJlaXRvIG7Do28tZXhjbHVzaXZvIGRlIHJlcHJvZHV6aXIsICB0cmFkdXppciAoY29uZm9ybWUgZGVmaW5pZG8gYWJhaXhvKSwgZS9vdQpkaXN0cmlidWlyIGEgc3VhIHRlc2Ugb3UgZGlzc2VydGHDp8OjbyAoaW5jbHVpbmRvIG8gcmVzdW1vKSBwb3IgdG9kbyBvIG11bmRvIG5vIGZvcm1hdG8gaW1wcmVzc28gZSBlbGV0csO0bmljbyBlCmVtIHF1YWxxdWVyIG1laW8sIGluY2x1aW5kbyBvcyBmb3JtYXRvcyDDoXVkaW8gb3UgdsOtZGVvLgoKVm9jw6ogY29uY29yZGEgcXVlIGEgVUZTQ2FyIHBvZGUsIHNlbSBhbHRlcmFyIG8gY29udGXDumRvLCB0cmFuc3BvciBhIHN1YSB0ZXNlIG91IGRpc3NlcnRhw6fDo28KcGFyYSBxdWFscXVlciBtZWlvIG91IGZvcm1hdG8gcGFyYSBmaW5zIGRlIHByZXNlcnZhw6fDo28uCgpWb2PDqiB0YW1iw6ltIGNvbmNvcmRhIHF1ZSBhIFVGU0NhciBwb2RlIG1hbnRlciBtYWlzIGRlIHVtYSBjw7NwaWEgYSBzdWEgdGVzZSBvdQpkaXNzZXJ0YcOnw6NvIHBhcmEgZmlucyBkZSBzZWd1cmFuw6dhLCBiYWNrLXVwIGUgcHJlc2VydmHDp8Ojby4KClZvY8OqIGRlY2xhcmEgcXVlIGEgc3VhIHRlc2Ugb3UgZGlzc2VydGHDp8OjbyDDqSBvcmlnaW5hbCBlIHF1ZSB2b2PDqiB0ZW0gbyBwb2RlciBkZSBjb25jZWRlciBvcyBkaXJlaXRvcyBjb250aWRvcwpuZXN0YSBsaWNlbsOnYS4gVm9jw6ogdGFtYsOpbSBkZWNsYXJhIHF1ZSBvIGRlcMOzc2l0byBkYSBzdWEgdGVzZSBvdSBkaXNzZXJ0YcOnw6NvIG7Do28sIHF1ZSBzZWphIGRlIHNldQpjb25oZWNpbWVudG8sIGluZnJpbmdlIGRpcmVpdG9zIGF1dG9yYWlzIGRlIG5pbmd1w6ltLgoKQ2FzbyBhIHN1YSB0ZXNlIG91IGRpc3NlcnRhw6fDo28gY29udGVuaGEgbWF0ZXJpYWwgcXVlIHZvY8OqIG7Do28gcG9zc3VpIGEgdGl0dWxhcmlkYWRlIGRvcyBkaXJlaXRvcyBhdXRvcmFpcywgdm9jw6oKZGVjbGFyYSBxdWUgb2J0ZXZlIGEgcGVybWlzc8OjbyBpcnJlc3RyaXRhIGRvIGRldGVudG9yIGRvcyBkaXJlaXRvcyBhdXRvcmFpcyBwYXJhIGNvbmNlZGVyIMOgIFVGU0NhcgpvcyBkaXJlaXRvcyBhcHJlc2VudGFkb3MgbmVzdGEgbGljZW7Dp2EsIGUgcXVlIGVzc2UgbWF0ZXJpYWwgZGUgcHJvcHJpZWRhZGUgZGUgdGVyY2Vpcm9zIGVzdMOhIGNsYXJhbWVudGUKaWRlbnRpZmljYWRvIGUgcmVjb25oZWNpZG8gbm8gdGV4dG8gb3Ugbm8gY29udGXDumRvIGRhIHRlc2Ugb3UgZGlzc2VydGHDp8OjbyBvcmEgZGVwb3NpdGFkYS4KCkNBU08gQSBURVNFIE9VIERJU1NFUlRBw4fDg08gT1JBIERFUE9TSVRBREEgVEVOSEEgU0lETyBSRVNVTFRBRE8gREUgVU0gUEFUUk9Dw41OSU8gT1UKQVBPSU8gREUgVU1BIEFHw4pOQ0lBIERFIEZPTUVOVE8gT1UgT1VUUk8gT1JHQU5JU01PIFFVRSBOw4NPIFNFSkEgQSBVRlNDYXIsClZPQ8OKIERFQ0xBUkEgUVVFIFJFU1BFSVRPVSBUT0RPUyBFIFFVQUlTUVVFUiBESVJFSVRPUyBERSBSRVZJU8ODTyBDT01PClRBTULDiU0gQVMgREVNQUlTIE9CUklHQcOHw5VFUyBFWElHSURBUyBQT1IgQ09OVFJBVE8gT1UgQUNPUkRPLgoKQSBVRlNDYXIgc2UgY29tcHJvbWV0ZSBhIGlkZW50aWZpY2FyIGNsYXJhbWVudGUgbyBzZXUgbm9tZSAocykgb3UgbyhzKSBub21lKHMpIGRvKHMpCmRldGVudG9yKGVzKSBkb3MgZGlyZWl0b3MgYXV0b3JhaXMgZGEgdGVzZSBvdSBkaXNzZXJ0YcOnw6NvLCBlIG7Do28gZmFyw6EgcXVhbHF1ZXIgYWx0ZXJhw6fDo28sIGFsw6ltIGRhcXVlbGFzCmNvbmNlZGlkYXMgcG9yIGVzdGEgbGljZW7Dp2EuCg==Repositório InstitucionalPUBhttps://repositorio.ufscar.br/oai/requestopendoar:43222023-05-25T12:56:12.502363Repositório Institucional da UFSCAR - Universidade Federal de São Carlos (UFSCAR)false |
dc.title.por.fl_str_mv |
Espectroscopia Raman amplificada por superfície associada à cromatografia em camada delgada para análise de amostras alimentícias |
dc.title.alternative.eng.fl_str_mv |
Surface enhancement Raman spectroscopy coupled to thin-layer chromatography for analysis of food samples |
dc.title.alternative.fre.fl_str_mv |
Diffusion Raman exaltée par effet de surface associée à chromatographie sur couche mince pour l'analyse d'échantillons alimentaires |
title |
Espectroscopia Raman amplificada por superfície associada à cromatografia em camada delgada para análise de amostras alimentícias |
spellingShingle |
Espectroscopia Raman amplificada por superfície associada à cromatografia em camada delgada para análise de amostras alimentícias Soares, Frederico Luis Felipe Quimiometria Cerveja Leite Vinho SERS TLC Chemometrics Beer Milk Wine CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA |
title_short |
Espectroscopia Raman amplificada por superfície associada à cromatografia em camada delgada para análise de amostras alimentícias |
title_full |
Espectroscopia Raman amplificada por superfície associada à cromatografia em camada delgada para análise de amostras alimentícias |
title_fullStr |
Espectroscopia Raman amplificada por superfície associada à cromatografia em camada delgada para análise de amostras alimentícias |
title_full_unstemmed |
Espectroscopia Raman amplificada por superfície associada à cromatografia em camada delgada para análise de amostras alimentícias |
title_sort |
Espectroscopia Raman amplificada por superfície associada à cromatografia em camada delgada para análise de amostras alimentícias |
author |
Soares, Frederico Luis Felipe |
author_facet |
Soares, Frederico Luis Felipe |
author_role |
author |
dc.contributor.authorlattes.por.fl_str_mv |
http://lattes.cnpq.br/1064620847107189 |
dc.contributor.author.fl_str_mv |
Soares, Frederico Luis Felipe |
dc.contributor.advisor1.fl_str_mv |
Carneiro, Renato Lajarim |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/8065852319463976 |
contributor_str_mv |
Carneiro, Renato Lajarim |
dc.subject.por.fl_str_mv |
Quimiometria Cerveja Leite Vinho SERS TLC |
topic |
Quimiometria Cerveja Leite Vinho SERS TLC Chemometrics Beer Milk Wine CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA |
dc.subject.eng.fl_str_mv |
Chemometrics Beer Milk Wine |
dc.subject.cnpq.fl_str_mv |
CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA |
description |
Surface enhancement Raman spectroscopy (SERS) presents the advantages of conventional Raman spectroscopy with the possibility to detect compounds in low levels due to the enhancement on Raman intensity, generated by the molecule-nanoparticle system. Thin-layer chromatography (TLC) is a fast and easy separation technique, that can be coupled to several analytical techniques in order to identify compounds. TLC-SERS is a relatively new technique, with only a few works published; however it presents the advantages of both techniques synergically. The use of nanoparticles adsorbed onto the TLC plate enables to obtain Raman spectra of the separated compounds even in low concentrations. Therefore, this work proposes the use of TLC-SERS in three different application of food interest: product authentication, food safety and stability studies. 1) In product authentication, it was analyzed Pilsner beer samples in order to obtain pattern recognition related to brand and brewery. Samples were prepared in TLC plates and sprayed with gold nanoparticle to promote SERS analysis regarding the elution line of the target analytes. The obtained results were compared by two chemometric methods of data decomposition and signal recovering: multivariate curve resolution (MCR) and independent component analysis (ICA). From the obtained chromatographic peaks was possible to perform fingerprint analysis and identify clustering pattern concerning sample brand and brewery location. 2) As food safety application, the aim was to develop and optimize an analytical methodology to quantify two veterinary drugs (sulfamethoxazole and trimethoprim) in bovine milk. Central composite design was applied evaluating NaCl concentration and nanoparticles pre-concentration to optimize the analytical signal. The hyperspectral images obtained from TLC-SERS were processed using different chemometric methods. For trimethoprim, it was obtained recoveries of 82 – 112% in milk samples. Due to the high complexity of the samples, it was not possible to obtain reliable quantitative values for sulfamethoxazole. 3) For the stability study, it was kinetically assessed one red wine sample under different degradation conditions. For this, it was used a 2³ design of experiments varying pH, dissolved O2 and the presence of anti-oxidant agent. Samples were left in three stocking temperatures (4, 24 and 40 °C) and evaluated during 45 days. SERS chromatograms were analyzed using ICA, and from the chromatographic profile, it was possible to perform ANOVA-PCA where it was identified temperature and the presence of anti-oxidant agent as the most significant variables. |
publishDate |
2018 |
dc.date.accessioned.fl_str_mv |
2018-07-11T11:51:02Z |
dc.date.available.fl_str_mv |
2018-07-11T11:51:02Z |
dc.date.issued.fl_str_mv |
2018-04-13 |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/doctoralThesis |
format |
doctoralThesis |
status_str |
publishedVersion |
dc.identifier.citation.fl_str_mv |
SOARES, Frederico Luis Felipe. Espectroscopia Raman amplificada por superfície associada à cromatografia em camada delgada para análise de amostras alimentícias. 2018. Tese (Doutorado em Química) – Universidade Federal de São Carlos, São Carlos, 2018. Disponível em: https://repositorio.ufscar.br/handle/ufscar/10272. |
dc.identifier.uri.fl_str_mv |
https://repositorio.ufscar.br/handle/ufscar/10272 |
identifier_str_mv |
SOARES, Frederico Luis Felipe. Espectroscopia Raman amplificada por superfície associada à cromatografia em camada delgada para análise de amostras alimentícias. 2018. Tese (Doutorado em Química) – Universidade Federal de São Carlos, São Carlos, 2018. Disponível em: https://repositorio.ufscar.br/handle/ufscar/10272. |
url |
https://repositorio.ufscar.br/handle/ufscar/10272 |
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por |
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openAccess |
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Universidade Federal de São Carlos Câmpus São Carlos |
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Programa de Pós-Graduação em Química - PPGQ |
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UFSCar |
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Universidade Federal de São Carlos Câmpus São Carlos |
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