Síntese, caracterização e aplicação de um polímero molecularmente impresso (MIP) com atividade catalítica para oxidação de epinefrina
| Ano de defesa: | 2010 |
|---|---|
| Autor(a) principal: | |
| Orientador(a): | |
| Banca de defesa: | , |
| Tipo de documento: | Dissertação |
| Tipo de acesso: | Acesso aberto |
| Idioma: | por |
| Instituição de defesa: |
Universidade Federal de Alfenas
|
| Programa de Pós-Graduação: |
Programa de Pós-Graduação em Ciências Farmacêuticas
|
| Departamento: |
Faculdade de Ciências Farmacêuticas
|
| País: |
Brasil
|
| Palavras-chave em Português: | |
| Área do conhecimento CNPq: | |
| Link de acesso: | https://repositorio.unifal-mg.edu.br/handle/123456789/727 |
Resumo: | The technique for preparation of molecularly imprinted polymers (MIP), since its first description in 1972, has promoted relevant advances to different segments of Analytical Chemistry, particularly in procedures for solid phase extraction. However, the use of imprinted polymers with catalytic activity is still young. In the present work was synthesized a MIP (MIP-MAA) with selective catalytic activity for the oxidation of epinephrine (EP) by hydrogen peroxide (H2O2) using hemin and methacrylic acid (MAA) as functional monomers in the synthesis of the polymer, giving to the MIP selective and prosthetic binding sites for the template molecule of EP and also increasing the activity of the material in water. Simultaneously were prepared the following materials: non-imprinted polymer (NIP1), non-imprinted polymer without hemin (NIP2) and imprinted polymer with hemin and 4-vinylpyridine (MIP-4VPy). The materials were synthesized using the technique of bulk by free radical polymerization thermo-activated, as described by Santos et al (2007) with minor modifications. After synthesis, the materials were milled, dried and sieved to a maximum diameter of 106 µm. Afterward, the template molecule was extracted from MIP with a solution of methanol: acetic acid (4:1) (v / v) and the final product was submitted to analysis of physical characterization, such as scanning electron microscopy (SEM), thermogravimetry (TG) and infrared (IR). The detection technique was amperometry with the potential fixed in 0.0 V vs. Ag / AgCl, which was coupled to the output of a system of flow injection analysis (FIA) in a single line mode. The FIA system consisted of the introduction of the sample EP (tris-HCl 0.1 mmol L-¹, pH 8.0, 120 µL) in a carrier stream of H2O2 (300 µmol L-¹, 0.9 mL min-¹). After percolation of the sample on the biomimetic reactor, the catalysis of the EP oxidation by H2O2 occur, being the product formed monitored by amperometry through the variation of current versus time. The MIP-MAA showed higher catalytic activity of NIP1, NIP2 and MIP-4VPy, demonstrating the effectiveness of molecular imprinting. The level of interference observed for molecules similar to the EP was less than 45% considering the signal amplitude. Through physical characterization was possible to detect the presence of morphological differences between the MIP-MAA, NIP1 and NIP2, especially in the TG analysis. |
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Sartori, Lucas Rossihttp://lattes.cnpq.br/9803419937796467Pereira, Arnaldo CésarFigueiredo, Eduardo Costa DeTarley, César Ricardo Teixeirahttp://lattes.cnpq.br/29805108410590572015-11-18T22:43:16Z2010-02-03SARTORI, Lucas Rossi. Síntese, caracterização e aplicação de um polímero molecularmente impresso (MIP) com atividade catalítica para oxidação de epinefrina. 2010. 101 f. Dissertação (mestrado em Ciências Farmacêuticas) - Universidade Federal de Alfenas, Alfenas, MG, 2010.https://repositorio.unifal-mg.edu.br/handle/123456789/727The technique for preparation of molecularly imprinted polymers (MIP), since its first description in 1972, has promoted relevant advances to different segments of Analytical Chemistry, particularly in procedures for solid phase extraction. However, the use of imprinted polymers with catalytic activity is still young. In the present work was synthesized a MIP (MIP-MAA) with selective catalytic activity for the oxidation of epinephrine (EP) by hydrogen peroxide (H2O2) using hemin and methacrylic acid (MAA) as functional monomers in the synthesis of the polymer, giving to the MIP selective and prosthetic binding sites for the template molecule of EP and also increasing the activity of the material in water. Simultaneously were prepared the following materials: non-imprinted polymer (NIP1), non-imprinted polymer without hemin (NIP2) and imprinted polymer with hemin and 4-vinylpyridine (MIP-4VPy). The materials were synthesized using the technique of bulk by free radical polymerization thermo-activated, as described by Santos et al (2007) with minor modifications. After synthesis, the materials were milled, dried and sieved to a maximum diameter of 106 µm. Afterward, the template molecule was extracted from MIP with a solution of methanol: acetic acid (4:1) (v / v) and the final product was submitted to analysis of physical characterization, such as scanning electron microscopy (SEM), thermogravimetry (TG) and infrared (IR). The detection technique was amperometry with the potential fixed in 0.0 V vs. Ag / AgCl, which was coupled to the output of a system of flow injection analysis (FIA) in a single line mode. The FIA system consisted of the introduction of the sample EP (tris-HCl 0.1 mmol L-¹, pH 8.0, 120 µL) in a carrier stream of H2O2 (300 µmol L-¹, 0.9 mL min-¹). After percolation of the sample on the biomimetic reactor, the catalysis of the EP oxidation by H2O2 occur, being the product formed monitored by amperometry through the variation of current versus time. The MIP-MAA showed higher catalytic activity of NIP1, NIP2 and MIP-4VPy, demonstrating the effectiveness of molecular imprinting. The level of interference observed for molecules similar to the EP was less than 45% considering the signal amplitude. Through physical characterization was possible to detect the presence of morphological differences between the MIP-MAA, NIP1 and NIP2, especially in the TG analysis.A técnica de preparação de polímeros molecularmente impressos (MIP), desde seu surgimento em 1972, tem promovido avanços relevantes em diferentes segmentos da Química Analítica, principalmente em procedimentos de extração em fase sólida. Porém, o uso de polímeros impressos com atividade catalítica ainda é recente. Assim, no presente trabalho foi sintetizado um MIP (MIP-MAA) seletivo com atividade catalítica na reação de oxidação de epinefrina (EP) por peróxido de hidrogênio (H2O2) utilizando hemina e ácido metacrílico (MAA) como monômeros funcionais na síntese do polímero, conferindo ao MIP sítios seletivos e prostéticos à molécula molde de EP e também aumentando a atividade do material em meio aquoso. Foram preparados simultaneamente: polímero não impresso (NIP1), polímero não impresso sem hemina (NIP2) e polímero impresso com hemina e 4-vinilpiridina (MIP-4VPy). Os materiais foram sintetizados utilizando-se a técnica de "bulk", através de polimerização radicalar livre termoativada, conforme descrito por Santos et al (2007) com pequenas modificações. Após a síntese, os materiais foram triturados, secos e peneirados em diâmetro máximo de 106 µm e na seqüência procedeu-se a extração da molécula molde com solução de metanol:ácido acético (4:1) (v/v). O material foi submetido a análises de caracterização física, como microscopia eletrônica de varredura (MEV), termogravimetria (TG) e infravermelho (IR). A técnica de detecção foi a amperometria com potencial fixo em 0,0 V vs Ag/AgCl, a qual foi acoplada à saída de um sistema de injeção em fluxo (FIA) de linha única. O sistema FIA consistiu da introdução da amostra de EP (tampão tris-HCl 0,1 mmol L-¹, pH 8,0, 120 µL) num fluxo carregador de H2O2 (300 µmol L-¹, 0,9 mL min-¹). Após percolação da amostra no reator biomimético, ocorre catálise da reação de oxidação da EP pelo H2O2, onde o produto formado é monitorado por amperometria através da variação de corrente versus tempo. O MIP-MAA demonstrou atividade catalítica superior ao NIP1, NIP2 e MIP-4VPy, evidenciado a efetividade da impressão molecular. O nível de interferência observado para moléculas semelhantes à EP foi inferior a 45% considerando-se a amplitude de sinal. Por meio da caracterização física foi possível detectar a presença de diferenças morfológicas entre o MIP-MAA, NIP1 e NIP2, principalmente na análise de TG.Fundação de Amparo à Pesquisa do Estado de Minas Gerais - FAPEMIGapplication/pdfporUniversidade Federal de AlfenasPrograma de Pós-Graduação em Ciências FarmacêuticasUNIFAL-MGBrasilFaculdade de Ciências Farmacêuticasinfo:eu-repo/semantics/openAccesshttp://creativecommons.org/licenses/by-nc-nd/4.0/EpinefrinaAnálise Química - MetodosImpressão MolecularPolímeros - químicaAnálise de injeção de FluxoCIENCIAS DA SAUDE::FARMACIASíntese, caracterização e aplicação de um polímero molecularmente impresso (MIP) com atividade catalítica para oxidação de epinefrinainfo:eu-repo/semantics/masterThesisinfo:eu-repo/semantics/publishedVersion-64258451559862442976006006006997636413449754996-1527361517405938873reponame:Repositório Institucional da Universidade Federal de Alfenas - RiUnifalinstname:Universidade Federal de Alfenas (UNIFAL)instacron:UNIFALSartori, Lucas RossiLICENSElicense.txtlicense.txttext/plain; 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| dc.title.pt-BR.fl_str_mv |
Síntese, caracterização e aplicação de um polímero molecularmente impresso (MIP) com atividade catalítica para oxidação de epinefrina |
| title |
Síntese, caracterização e aplicação de um polímero molecularmente impresso (MIP) com atividade catalítica para oxidação de epinefrina |
| spellingShingle |
Síntese, caracterização e aplicação de um polímero molecularmente impresso (MIP) com atividade catalítica para oxidação de epinefrina Sartori, Lucas Rossi Epinefrina Análise Química - Metodos Impressão Molecular Polímeros - química Análise de injeção de Fluxo CIENCIAS DA SAUDE::FARMACIA |
| title_short |
Síntese, caracterização e aplicação de um polímero molecularmente impresso (MIP) com atividade catalítica para oxidação de epinefrina |
| title_full |
Síntese, caracterização e aplicação de um polímero molecularmente impresso (MIP) com atividade catalítica para oxidação de epinefrina |
| title_fullStr |
Síntese, caracterização e aplicação de um polímero molecularmente impresso (MIP) com atividade catalítica para oxidação de epinefrina |
| title_full_unstemmed |
Síntese, caracterização e aplicação de um polímero molecularmente impresso (MIP) com atividade catalítica para oxidação de epinefrina |
| title_sort |
Síntese, caracterização e aplicação de um polímero molecularmente impresso (MIP) com atividade catalítica para oxidação de epinefrina |
| author |
Sartori, Lucas Rossi |
| author_facet |
Sartori, Lucas Rossi |
| author_role |
author |
| dc.contributor.author.fl_str_mv |
Sartori, Lucas Rossi |
| dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/9803419937796467 |
| dc.contributor.referee1.fl_str_mv |
Pereira, Arnaldo César |
| dc.contributor.referee2.fl_str_mv |
Figueiredo, Eduardo Costa De |
| dc.contributor.advisor1.fl_str_mv |
Tarley, César Ricardo Teixeira |
| dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/2980510841059057 |
| contributor_str_mv |
Pereira, Arnaldo César Figueiredo, Eduardo Costa De Tarley, César Ricardo Teixeira |
| dc.subject.por.fl_str_mv |
Epinefrina Análise Química - Metodos Impressão Molecular Polímeros - química Análise de injeção de Fluxo |
| topic |
Epinefrina Análise Química - Metodos Impressão Molecular Polímeros - química Análise de injeção de Fluxo CIENCIAS DA SAUDE::FARMACIA |
| dc.subject.cnpq.fl_str_mv |
CIENCIAS DA SAUDE::FARMACIA |
| description |
The technique for preparation of molecularly imprinted polymers (MIP), since its first description in 1972, has promoted relevant advances to different segments of Analytical Chemistry, particularly in procedures for solid phase extraction. However, the use of imprinted polymers with catalytic activity is still young. In the present work was synthesized a MIP (MIP-MAA) with selective catalytic activity for the oxidation of epinephrine (EP) by hydrogen peroxide (H2O2) using hemin and methacrylic acid (MAA) as functional monomers in the synthesis of the polymer, giving to the MIP selective and prosthetic binding sites for the template molecule of EP and also increasing the activity of the material in water. Simultaneously were prepared the following materials: non-imprinted polymer (NIP1), non-imprinted polymer without hemin (NIP2) and imprinted polymer with hemin and 4-vinylpyridine (MIP-4VPy). The materials were synthesized using the technique of bulk by free radical polymerization thermo-activated, as described by Santos et al (2007) with minor modifications. After synthesis, the materials were milled, dried and sieved to a maximum diameter of 106 µm. Afterward, the template molecule was extracted from MIP with a solution of methanol: acetic acid (4:1) (v / v) and the final product was submitted to analysis of physical characterization, such as scanning electron microscopy (SEM), thermogravimetry (TG) and infrared (IR). The detection technique was amperometry with the potential fixed in 0.0 V vs. Ag / AgCl, which was coupled to the output of a system of flow injection analysis (FIA) in a single line mode. The FIA system consisted of the introduction of the sample EP (tris-HCl 0.1 mmol L-¹, pH 8.0, 120 µL) in a carrier stream of H2O2 (300 µmol L-¹, 0.9 mL min-¹). After percolation of the sample on the biomimetic reactor, the catalysis of the EP oxidation by H2O2 occur, being the product formed monitored by amperometry through the variation of current versus time. The MIP-MAA showed higher catalytic activity of NIP1, NIP2 and MIP-4VPy, demonstrating the effectiveness of molecular imprinting. The level of interference observed for molecules similar to the EP was less than 45% considering the signal amplitude. Through physical characterization was possible to detect the presence of morphological differences between the MIP-MAA, NIP1 and NIP2, especially in the TG analysis. |
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2010 |
| dc.date.issued.fl_str_mv |
2010-02-03 |
| dc.date.accessioned.fl_str_mv |
2015-11-18T22:43:16Z |
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info:eu-repo/semantics/masterThesis |
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info:eu-repo/semantics/publishedVersion |
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masterThesis |
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publishedVersion |
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SARTORI, Lucas Rossi. Síntese, caracterização e aplicação de um polímero molecularmente impresso (MIP) com atividade catalítica para oxidação de epinefrina. 2010. 101 f. Dissertação (mestrado em Ciências Farmacêuticas) - Universidade Federal de Alfenas, Alfenas, MG, 2010. |
| dc.identifier.uri.fl_str_mv |
https://repositorio.unifal-mg.edu.br/handle/123456789/727 |
| identifier_str_mv |
SARTORI, Lucas Rossi. Síntese, caracterização e aplicação de um polímero molecularmente impresso (MIP) com atividade catalítica para oxidação de epinefrina. 2010. 101 f. Dissertação (mestrado em Ciências Farmacêuticas) - Universidade Federal de Alfenas, Alfenas, MG, 2010. |
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por |
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por |
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600 600 600 |
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info:eu-repo/semantics/openAccess http://creativecommons.org/licenses/by-nc-nd/4.0/ |
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openAccess |
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http://creativecommons.org/licenses/by-nc-nd/4.0/ |
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Universidade Federal de Alfenas |
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Programa de Pós-Graduação em Ciências Farmacêuticas |
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UNIFAL-MG |
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Brasil |
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Faculdade de Ciências Farmacêuticas |
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Universidade Federal de Alfenas |
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Repositório Institucional da Universidade Federal de Alfenas - RiUnifal |
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| bitstream.checksumAlgorithm.fl_str_mv |
MD5 MD5 MD5 MD5 MD5 MD5 MD5 |
| repository.name.fl_str_mv |
Repositório Institucional da Universidade Federal de Alfenas - RiUnifal - Universidade Federal de Alfenas (UNIFAL) |
| repository.mail.fl_str_mv |
repositorio@unifal-mg.edu.br |
| _version_ |
1859830877516726272 |