Polímero de impressão molecular sintetizado por micro-ondas para extração em fase sólida e quantificação de cocaína em amostras ambientais
| Ano de defesa: | 2021 |
|---|---|
| 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 Engenharia Química
|
| Departamento: |
Instituto de Ciência e Tecnologia
|
| País: |
Brasil
|
| Palavras-chave em Português: | |
| Área do conhecimento CNPq: | |
| Link de acesso: | https://repositorio.unifal-mg.edu.br/handle/123456789/2062 |
Resumo: | Cocaine is an illicit drug of abuse that causes numerous social problems and the measurement of its consumption by the population requires more precise methodologies for quantification in different environmental samples and one of the ways is the quantification of the metabolites or original molecules in the sewage network. The solid phase extraction (SPE) technique using molecular imprinting polymer (MIP) as solid phase (MISPE) is a technique that allows to eliminate the interferences from the matrix and concentrate the sample. Therefore, MIPs were synthesized using microwave energy (MW) in different parameters for use in MISPE. The polymers were produced in powers of 80W and 100W and in the range of 15 to 60 minutes of reaction time. After the synthesis, the mass yield, molecular structure, thermal stability and surface area were analyzed. Then, two polymers synthesized with the cocaine as template molecule (MIP-1C and MIP-10C) were compared and finally the MIP-10C was used to quantify cocaine in urban sewage in the city of Poços de Caldas (MG). The results obtained showed a mass yield of more than 90% for the addition of Cocaine as a target molecule when compared to the polymer without addition of a template molecule and an increase in mass yield of 39% for adjustments only in the synthesis potency. In all analyzed polymers, the incorporation of the cross-linker into the polymer structure and the alteration of the chemical structure with the addition of the template molecule was demonstrated by the FTIR technique. The thermal stability was determined up to 120 ºC and when increasing the synthesis power to 100W, the polymer was synthesized after 15 minutes and at 80W there was a 65% increase in the surface area (BET) when compared to the power of 100W. The best synthesis results were obtained at 80W of power and 30 minutes of reaction time. The MIP adsorption and desorption tests showed an adsorption capacity of cocaine from the aqueous medium of 1.37% of the polymer weight, a recovery rate of 90% and the analysis of urban sewage estimated a monthly population consumption in Poços de Caldas (MG) of approximately 1,113 kg of powder containing cocaine. |
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Shinma, Renê Arrierohttp://lattes.cnpq.br/7759622872412835Bertholdo, Robertohttp://lattes.cnpq.br/2682000754706724Moreira, Ailton JoséFigueiredo, Eduardo Costa DeFreschi, Gian Paulo Giovannihttp://lattes.cnpq.br/50888601430179062022-07-12T23:16:31Z2021-12-16SHINMA, Renê Arriero. Polímero de impressão molecular sintetizado por micro-ondas para extração em fase sólida e quantificação de cocaína em amostras ambientais. 2021. 102 f. Dissertação (Mestrado em Engenharia Química) - Universidade Federal de Alfenas, Poços de Caldas, MG, 2021.https://repositorio.unifal-mg.edu.br/handle/123456789/2062Cocaine is an illicit drug of abuse that causes numerous social problems and the measurement of its consumption by the population requires more precise methodologies for quantification in different environmental samples and one of the ways is the quantification of the metabolites or original molecules in the sewage network. The solid phase extraction (SPE) technique using molecular imprinting polymer (MIP) as solid phase (MISPE) is a technique that allows to eliminate the interferences from the matrix and concentrate the sample. Therefore, MIPs were synthesized using microwave energy (MW) in different parameters for use in MISPE. The polymers were produced in powers of 80W and 100W and in the range of 15 to 60 minutes of reaction time. After the synthesis, the mass yield, molecular structure, thermal stability and surface area were analyzed. Then, two polymers synthesized with the cocaine as template molecule (MIP-1C and MIP-10C) were compared and finally the MIP-10C was used to quantify cocaine in urban sewage in the city of Poços de Caldas (MG). The results obtained showed a mass yield of more than 90% for the addition of Cocaine as a target molecule when compared to the polymer without addition of a template molecule and an increase in mass yield of 39% for adjustments only in the synthesis potency. In all analyzed polymers, the incorporation of the cross-linker into the polymer structure and the alteration of the chemical structure with the addition of the template molecule was demonstrated by the FTIR technique. The thermal stability was determined up to 120 ºC and when increasing the synthesis power to 100W, the polymer was synthesized after 15 minutes and at 80W there was a 65% increase in the surface area (BET) when compared to the power of 100W. The best synthesis results were obtained at 80W of power and 30 minutes of reaction time. The MIP adsorption and desorption tests showed an adsorption capacity of cocaine from the aqueous medium of 1.37% of the polymer weight, a recovery rate of 90% and the analysis of urban sewage estimated a monthly population consumption in Poços de Caldas (MG) of approximately 1,113 kg of powder containing cocaine.A cocaína é uma droga de abuso ilícita que causa inúmeros problemas sociais e a mensuração do seu consumo pela população exige metodologias mais precisas para quantificação em diferentes amostras ambientais e uma das formas é a quantificação dos metabólitos ou moléculas originais na rede de esgoto. A técnica de extração em fase sólida (SPE) utilizando polímero de impressão molecular (MIP) como fase sólida (MISPE) é uma técnica que permite eliminar os interferentes da matriz e concentrar a amostra. Portanto foram sintetizados MIPs utilizando energia micro-ondas (MW) em diferentes parâmetros para utilização em MISPE. Os polímeros foram produzidos em potências de 80W e 100W e no intervalo de 15 a 60 minutos de tempo de reação. Após a síntese foram analisados o rendimento em massa, estrutura molecular, estabilidade térmica e área superficial. Em seguida dois polímeros sintetizados com a molécula-molde de cocaína (MIP-1C e MIP-10C) foram comparados e por último o MIP-10C foi utilizado para quantificação de cocaína em esgoto urbano da cidade de Poços de Caldas (MG). Os resultados obtidos apresentaram um rendimento em massa de mais de 90% para adição de Cocaína como molécula-alvo quando comparado ao polímero sem adição de molécula-molde e um aumento no rendimento em massa de 39% para ajustes apenas na potência de síntese. Em todos os polímeros analisados foi demonstrado pela técnica de FTIR a incorporação do ligante cruzado na estrutura do polímero e a alteração da estrutura química com a adição da molécula-molde. A estabilidade térmica foi determinada até 120 ºC e ao aumentar a potência de síntese para 100W houve a síntese do polímero a partir de 15 minutos e em 80W houve um aumento de 65% da área superficial (BET) quando comparado à potência de 100W. Os melhores resultados de síntese foram obtidos em 80W de potência e 30 minutos de tempo de reação. Os testes de adsorção e dessorção do MIP demonstraram uma capacidade de adsorção de cocaína do meio aquoso de 1,37% do peso do polímero, uma taxa de recuperação de 90% e a análise do esgoto urbano estimou um consumo populacional mensal em Poços de Caldas (MG) de aproximadamente 1,113Kg de pó contendo cocaína.application/pdfporUniversidade Federal de AlfenasPrograma de Pós-Graduação em Engenharia QuímicaUNIFAL-MGBrasilInstituto de Ciência e Tecnologiainfo:eu-repo/semantics/openAccesshttp://creativecommons.org/licenses/by-nc-nd/4.0/Cocaína.Polímeros de impressão molecular.Energia microondas.SPE.Amostras ambientais.ENGENHARIASPolímero de impressão molecular sintetizado por micro-ondas para extração em fase sólida e quantificação de cocaína em amostras ambientaisMicrowave-synthesized molecular imprint polymer for solid phase extraction and quantification of cocaine in environmental samplesinfo:eu-repo/semantics/masterThesisinfo:eu-repo/semantics/publishedVersion-42974172594986389316006004518971056484826825reponame:Repositório Institucional da Universidade Federal de Alfenas - RiUnifalinstname:Universidade Federal de Alfenas (UNIFAL)instacron:UNIFALShinma, Renê ArrieroLICENSElicense.txtlicense.txttext/plain; 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| dc.title.pt-BR.fl_str_mv |
Polímero de impressão molecular sintetizado por micro-ondas para extração em fase sólida e quantificação de cocaína em amostras ambientais |
| dc.title.alternative.eng.fl_str_mv |
Microwave-synthesized molecular imprint polymer for solid phase extraction and quantification of cocaine in environmental samples |
| title |
Polímero de impressão molecular sintetizado por micro-ondas para extração em fase sólida e quantificação de cocaína em amostras ambientais |
| spellingShingle |
Polímero de impressão molecular sintetizado por micro-ondas para extração em fase sólida e quantificação de cocaína em amostras ambientais Shinma, Renê Arriero Cocaína. Polímeros de impressão molecular. Energia microondas. SPE. Amostras ambientais. ENGENHARIAS |
| title_short |
Polímero de impressão molecular sintetizado por micro-ondas para extração em fase sólida e quantificação de cocaína em amostras ambientais |
| title_full |
Polímero de impressão molecular sintetizado por micro-ondas para extração em fase sólida e quantificação de cocaína em amostras ambientais |
| title_fullStr |
Polímero de impressão molecular sintetizado por micro-ondas para extração em fase sólida e quantificação de cocaína em amostras ambientais |
| title_full_unstemmed |
Polímero de impressão molecular sintetizado por micro-ondas para extração em fase sólida e quantificação de cocaína em amostras ambientais |
| title_sort |
Polímero de impressão molecular sintetizado por micro-ondas para extração em fase sólida e quantificação de cocaína em amostras ambientais |
| author |
Shinma, Renê Arriero |
| author_facet |
Shinma, Renê Arriero |
| author_role |
author |
| dc.contributor.author.fl_str_mv |
Shinma, Renê Arriero |
| dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/7759622872412835 |
| dc.contributor.advisor-co1.fl_str_mv |
Bertholdo, Roberto |
| dc.contributor.advisor-co1Lattes.fl_str_mv |
http://lattes.cnpq.br/2682000754706724 |
| dc.contributor.referee1.fl_str_mv |
Moreira, Ailton José |
| dc.contributor.referee2.fl_str_mv |
Figueiredo, Eduardo Costa De |
| dc.contributor.advisor1.fl_str_mv |
Freschi, Gian Paulo Giovanni |
| dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/5088860143017906 |
| contributor_str_mv |
Bertholdo, Roberto Moreira, Ailton José Figueiredo, Eduardo Costa De Freschi, Gian Paulo Giovanni |
| dc.subject.por.fl_str_mv |
Cocaína. Polímeros de impressão molecular. Energia microondas. SPE. Amostras ambientais. |
| topic |
Cocaína. Polímeros de impressão molecular. Energia microondas. SPE. Amostras ambientais. ENGENHARIAS |
| dc.subject.cnpq.fl_str_mv |
ENGENHARIAS |
| description |
Cocaine is an illicit drug of abuse that causes numerous social problems and the measurement of its consumption by the population requires more precise methodologies for quantification in different environmental samples and one of the ways is the quantification of the metabolites or original molecules in the sewage network. The solid phase extraction (SPE) technique using molecular imprinting polymer (MIP) as solid phase (MISPE) is a technique that allows to eliminate the interferences from the matrix and concentrate the sample. Therefore, MIPs were synthesized using microwave energy (MW) in different parameters for use in MISPE. The polymers were produced in powers of 80W and 100W and in the range of 15 to 60 minutes of reaction time. After the synthesis, the mass yield, molecular structure, thermal stability and surface area were analyzed. Then, two polymers synthesized with the cocaine as template molecule (MIP-1C and MIP-10C) were compared and finally the MIP-10C was used to quantify cocaine in urban sewage in the city of Poços de Caldas (MG). The results obtained showed a mass yield of more than 90% for the addition of Cocaine as a target molecule when compared to the polymer without addition of a template molecule and an increase in mass yield of 39% for adjustments only in the synthesis potency. In all analyzed polymers, the incorporation of the cross-linker into the polymer structure and the alteration of the chemical structure with the addition of the template molecule was demonstrated by the FTIR technique. The thermal stability was determined up to 120 ºC and when increasing the synthesis power to 100W, the polymer was synthesized after 15 minutes and at 80W there was a 65% increase in the surface area (BET) when compared to the power of 100W. The best synthesis results were obtained at 80W of power and 30 minutes of reaction time. The MIP adsorption and desorption tests showed an adsorption capacity of cocaine from the aqueous medium of 1.37% of the polymer weight, a recovery rate of 90% and the analysis of urban sewage estimated a monthly population consumption in Poços de Caldas (MG) of approximately 1,113 kg of powder containing cocaine. |
| publishDate |
2021 |
| dc.date.issued.fl_str_mv |
2021-12-16 |
| dc.date.accessioned.fl_str_mv |
2022-07-12T23:16:31Z |
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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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SHINMA, Renê Arriero. Polímero de impressão molecular sintetizado por micro-ondas para extração em fase sólida e quantificação de cocaína em amostras ambientais. 2021. 102 f. Dissertação (Mestrado em Engenharia Química) - Universidade Federal de Alfenas, Poços de Caldas, MG, 2021. |
| dc.identifier.uri.fl_str_mv |
https://repositorio.unifal-mg.edu.br/handle/123456789/2062 |
| identifier_str_mv |
SHINMA, Renê Arriero. Polímero de impressão molecular sintetizado por micro-ondas para extração em fase sólida e quantificação de cocaína em amostras ambientais. 2021. 102 f. Dissertação (Mestrado em Engenharia Química) - Universidade Federal de Alfenas, Poços de Caldas, MG, 2021. |
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por |
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por |
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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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application/pdf |
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Universidade Federal de Alfenas |
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UNIFAL-MG |
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Brasil |
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Instituto de Ciência e Tecnologia |
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Universidade Federal de Alfenas |
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31555718c4fc75849dd08f27935d4f6b 4afdbb8c545fd630ea7db775da747b2f d41d8cd98f00b204e9800998ecf8427e d41d8cd98f00b204e9800998ecf8427e d40fab288b703d01b6889f3d09475d1e eb481d06cf4b59a75151a969b8b951f3 a02a8051654caa789fdd228dda7a9836 |
| 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_ |
1859830870834151424 |