Espectrometria de massas por probe electrospray ionization (PESI-MS) com polímero molecularmente impresso (MIP) para determinação de ésteres de forbol em folhas de Jatropha curcas

Detalhes bibliográficos
Ano de defesa: 2018
Autor(a) principal: Silva, Lidya Cardozo da lattes
Orientador(a): Vaz, Boniek Gontijo lattes
Banca de defesa: Vaz, Boniek Gontijo, Terezan, Ana Paula, Kato, Lucília
Tipo de documento: Dissertação
Tipo de acesso: Acesso aberto
Idioma: por
Instituição de defesa: Universidade Federal de Goiás
Programa de Pós-Graduação: Programa de Pós-graduação em Química (IQ)
Departamento: Instituto de Química - IQ (RG)
País: Brasil
Palavras-chave em Português:
Palavras-chave em Inglês:
Área do conhecimento CNPq:
Link de acesso: http://repositorio.bc.ufg.br/tede/handle/tede/8813
Resumo: Jatropha curcas L. is a euphorbiaceous oilseed plant considered toxic to humans and animals due to the presence of phorbol esters (PEs). Traditionally, the detection of these toxic compounds has been done in J. curcas seeds and derivates via chromatographic separation methods such as HPLC-UV and HPLC-MS. Although efficient, these techniques are laborious and require high time and solvent consumption, thus it would be interesting the development of new analytical methods to determine these compounds with more practicality. Probe electrospray ionization is frequently used in ambient mass spectrometry allowing analysis with minimum sample preparation. However, for complex samples analysis, this technique presents low sensitivity and ionization suppression. In this study, a molecularly imprinted polymer-coated probe electrospray ionization mass spectrometry (MIPCPESI-MS) method was developed for determination of phorbol esters in methanolic extracts of Jatropha curcas leaves with direct extraction form the ionization source. The synthesized molecularly imprinted polymer (MIP) proved to be adequate for extraction of the PEs in methanolic extracts of J. curcas leaves with better performance as extraction phase in comparison with the non-imprinted polymer (NIP). The MIPCPESI method allowed detection of phorbol 12,13-diacetate (PDA) and other three PEs metabolite ions from Jatropha leaves with minimal sample preparation, and with higher signal intensities compared to analysis with conventional PESI. For the PDA, calibration curve exhibited linearity with R2 > 0.99, LOD and LOQ in µg.mL-1 range, precision and accuracy values, respectively, between 4.06 to 13.49% and -1.60 to -15.26 %. Finally, MIPCPESI was employed for PDA quantification in methanolic extracts of six different J. curcas leaves genotypes resulting in concentrations ranging from 222.19 ± 23.55 to 528.23 ± 19.72 µg.g-1 for toxic samples.
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spelling Vaz, Boniek Gontijohttp://lattes.cnpq.br/7814534710550639Vaz, Boniek GontijoTerezan, Ana PaulaKato, Lucíliahttp://lattes.cnpq.br/0226493098445253Silva, Lidya Cardozo da2018-08-20T13:38:04Z2018-07-20SILVA, L. C. Espectrometria de massas por probe electrospray ionization (PESI-MS) com polímero molecularmente impresso (MIP) para determinação de ésteres de forbol em folhas de Jatropha curcas. 2018. 45 f. Dissertação (Mestrado em Química) - Universidade Federal de Goiás, Goiânia, 2018.http://repositorio.bc.ufg.br/tede/handle/tede/8813Jatropha curcas L. is a euphorbiaceous oilseed plant considered toxic to humans and animals due to the presence of phorbol esters (PEs). Traditionally, the detection of these toxic compounds has been done in J. curcas seeds and derivates via chromatographic separation methods such as HPLC-UV and HPLC-MS. Although efficient, these techniques are laborious and require high time and solvent consumption, thus it would be interesting the development of new analytical methods to determine these compounds with more practicality. Probe electrospray ionization is frequently used in ambient mass spectrometry allowing analysis with minimum sample preparation. However, for complex samples analysis, this technique presents low sensitivity and ionization suppression. In this study, a molecularly imprinted polymer-coated probe electrospray ionization mass spectrometry (MIPCPESI-MS) method was developed for determination of phorbol esters in methanolic extracts of Jatropha curcas leaves with direct extraction form the ionization source. The synthesized molecularly imprinted polymer (MIP) proved to be adequate for extraction of the PEs in methanolic extracts of J. curcas leaves with better performance as extraction phase in comparison with the non-imprinted polymer (NIP). The MIPCPESI method allowed detection of phorbol 12,13-diacetate (PDA) and other three PEs metabolite ions from Jatropha leaves with minimal sample preparation, and with higher signal intensities compared to analysis with conventional PESI. For the PDA, calibration curve exhibited linearity with R2 > 0.99, LOD and LOQ in µg.mL-1 range, precision and accuracy values, respectively, between 4.06 to 13.49% and -1.60 to -15.26 %. Finally, MIPCPESI was employed for PDA quantification in methanolic extracts of six different J. curcas leaves genotypes resulting in concentrations ranging from 222.19 ± 23.55 to 528.23 ± 19.72 µg.g-1 for toxic samples.A Jatropha curcas L. é uma oleaginosa euforbiácea considerada tóxica para humanos e animais devido à presença de ésteres de forbol (PEs). Tradicionalmente, a detecção destes compostos tóxicos tem sido feita em tortas e sementes de J. curcas por meio do uso de técnicas de separação cromatográfica como HPLC-UV e HPLC-MS que apesar de eficientes são laboriosas e requerem alto consumo de tempo e solventes. Dessa forma, seria interessante o desenvolvimento de novas técnicas analíticas para determinação desses compostos com maior praticidade. Probe electrosrpay ionization (PESI) é uma das técnicas de ionização utilizadas na espectrometria de massas ambiente que permite análises rápidas com mínimo preparo de amostras. No entanto, para análise de amostras complexas essa técnica apresenta baixa sensibilidade e supressão iônica. Neste estudo, foi desenvolvido um método de análise por espectrometria de massas por Probe electrospray revestido com polímero molecularmente impresso (MIPCPESI-MS) para determinação de ésteres de forbol em extratos metanólicos de folhas de Jatropha curcas com extração direta da fonte de ionização. O polímero molecularmente impresso (MIP) sintetizado mostrou-se adequado para extração de PEs em extratos metanólicos de folhas de J. curcas tendo melhor desempenho como fase extratora quando comparado ao polímero não molecularmente impresso (NIP). O método MIPCPESI-MS possibilitou a detecção do forbol 12,13-diacetato (PDA) e de outros três íons metabólitos presentes nas folhas de J. curcas com mínimo preparo de amostras e com maior intensidade de sinais quando comparado às análises com PESI convencional. Para o PDA, a curva de calibração apresentou linearidade com R2 > 0.99, LOD e LOQ na faixa de µg.mL-1, valores de precisão entre 4.06 e 13.49 % e exatidão entre -1.60 e -15.26 %. Posteriormente, o método MIPCPESI foi empregado na quantificação de PDA em seis extratos metanólicos de diferentes genótipos de folhas de J. curcas resultando em valores concentrações entre 222.19 ± 23.55 a 528.23 ± 19.72 µg.g-1 nas amostras tóxicas.Submitted by Luciana Ferreira (lucgeral@gmail.com) on 2018-08-20T13:36:48Z No. of bitstreams: 2 Dissertação - Lidya Cardozo da Silva - 2018.pdf: 2382834 bytes, checksum: e5a79619d923d442540c5bf0549318bd (MD5) license_rdf: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5)Approved for entry into archive by Luciana Ferreira (lucgeral@gmail.com) on 2018-08-20T13:38:04Z (GMT) No. of bitstreams: 2 Dissertação - Lidya Cardozo da Silva - 2018.pdf: 2382834 bytes, checksum: e5a79619d923d442540c5bf0549318bd (MD5) license_rdf: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5)Made available in DSpace on 2018-08-20T13:38:04Z (GMT). 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dc.title.eng.fl_str_mv Espectrometria de massas por probe electrospray ionization (PESI-MS) com polímero molecularmente impresso (MIP) para determinação de ésteres de forbol em folhas de Jatropha curcas
dc.title.alternative.eng.fl_str_mv Molecularly imprinted polymer-coated probe electrospray ionization mass spectrometry (MIPCPESI-MS) for determination of phorbol esters in Jatropha curcas leaves
title Espectrometria de massas por probe electrospray ionization (PESI-MS) com polímero molecularmente impresso (MIP) para determinação de ésteres de forbol em folhas de Jatropha curcas
spellingShingle Espectrometria de massas por probe electrospray ionization (PESI-MS) com polímero molecularmente impresso (MIP) para determinação de ésteres de forbol em folhas de Jatropha curcas
Silva, Lidya Cardozo da
Espectrometria de massas ambiente
Probe electrospray ionization
Polímero molecularmente impresso
Jatropha curcas
Ésteres de forbol
Ambient mass spectrometry
Probe electrospray ionization
Molecularly imprinted polymer
Jatropha curcas
Phorbol esters
CIENCIAS EXATAS E DA TERRA::QUIMICA
title_short Espectrometria de massas por probe electrospray ionization (PESI-MS) com polímero molecularmente impresso (MIP) para determinação de ésteres de forbol em folhas de Jatropha curcas
title_full Espectrometria de massas por probe electrospray ionization (PESI-MS) com polímero molecularmente impresso (MIP) para determinação de ésteres de forbol em folhas de Jatropha curcas
title_fullStr Espectrometria de massas por probe electrospray ionization (PESI-MS) com polímero molecularmente impresso (MIP) para determinação de ésteres de forbol em folhas de Jatropha curcas
title_full_unstemmed Espectrometria de massas por probe electrospray ionization (PESI-MS) com polímero molecularmente impresso (MIP) para determinação de ésteres de forbol em folhas de Jatropha curcas
title_sort Espectrometria de massas por probe electrospray ionization (PESI-MS) com polímero molecularmente impresso (MIP) para determinação de ésteres de forbol em folhas de Jatropha curcas
author Silva, Lidya Cardozo da
author_facet Silva, Lidya Cardozo da
author_role author
dc.contributor.advisor1.fl_str_mv Vaz, Boniek Gontijo
dc.contributor.advisor1Lattes.fl_str_mv http://lattes.cnpq.br/7814534710550639
dc.contributor.referee1.fl_str_mv Vaz, Boniek Gontijo
dc.contributor.referee2.fl_str_mv Terezan, Ana Paula
dc.contributor.referee3.fl_str_mv Kato, Lucília
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/0226493098445253
dc.contributor.author.fl_str_mv Silva, Lidya Cardozo da
contributor_str_mv Vaz, Boniek Gontijo
Vaz, Boniek Gontijo
Terezan, Ana Paula
Kato, Lucília
dc.subject.por.fl_str_mv Espectrometria de massas ambiente
Probe electrospray ionization
Polímero molecularmente impresso
Jatropha curcas
Ésteres de forbol
topic Espectrometria de massas ambiente
Probe electrospray ionization
Polímero molecularmente impresso
Jatropha curcas
Ésteres de forbol
Ambient mass spectrometry
Probe electrospray ionization
Molecularly imprinted polymer
Jatropha curcas
Phorbol esters
CIENCIAS EXATAS E DA TERRA::QUIMICA
dc.subject.eng.fl_str_mv Ambient mass spectrometry
Probe electrospray ionization
Molecularly imprinted polymer
Jatropha curcas
Phorbol esters
dc.subject.cnpq.fl_str_mv CIENCIAS EXATAS E DA TERRA::QUIMICA
description Jatropha curcas L. is a euphorbiaceous oilseed plant considered toxic to humans and animals due to the presence of phorbol esters (PEs). Traditionally, the detection of these toxic compounds has been done in J. curcas seeds and derivates via chromatographic separation methods such as HPLC-UV and HPLC-MS. Although efficient, these techniques are laborious and require high time and solvent consumption, thus it would be interesting the development of new analytical methods to determine these compounds with more practicality. Probe electrospray ionization is frequently used in ambient mass spectrometry allowing analysis with minimum sample preparation. However, for complex samples analysis, this technique presents low sensitivity and ionization suppression. In this study, a molecularly imprinted polymer-coated probe electrospray ionization mass spectrometry (MIPCPESI-MS) method was developed for determination of phorbol esters in methanolic extracts of Jatropha curcas leaves with direct extraction form the ionization source. The synthesized molecularly imprinted polymer (MIP) proved to be adequate for extraction of the PEs in methanolic extracts of J. curcas leaves with better performance as extraction phase in comparison with the non-imprinted polymer (NIP). The MIPCPESI method allowed detection of phorbol 12,13-diacetate (PDA) and other three PEs metabolite ions from Jatropha leaves with minimal sample preparation, and with higher signal intensities compared to analysis with conventional PESI. For the PDA, calibration curve exhibited linearity with R2 > 0.99, LOD and LOQ in µg.mL-1 range, precision and accuracy values, respectively, between 4.06 to 13.49% and -1.60 to -15.26 %. Finally, MIPCPESI was employed for PDA quantification in methanolic extracts of six different J. curcas leaves genotypes resulting in concentrations ranging from 222.19 ± 23.55 to 528.23 ± 19.72 µg.g-1 for toxic samples.
publishDate 2018
dc.date.accessioned.fl_str_mv 2018-08-20T13:38:04Z
dc.date.issued.fl_str_mv 2018-07-20
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
dc.type.driver.fl_str_mv info:eu-repo/semantics/masterThesis
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dc.identifier.citation.fl_str_mv SILVA, L. C. Espectrometria de massas por probe electrospray ionization (PESI-MS) com polímero molecularmente impresso (MIP) para determinação de ésteres de forbol em folhas de Jatropha curcas. 2018. 45 f. Dissertação (Mestrado em Química) - Universidade Federal de Goiás, Goiânia, 2018.
dc.identifier.uri.fl_str_mv http://repositorio.bc.ufg.br/tede/handle/tede/8813
identifier_str_mv SILVA, L. C. Espectrometria de massas por probe electrospray ionization (PESI-MS) com polímero molecularmente impresso (MIP) para determinação de ésteres de forbol em folhas de Jatropha curcas. 2018. 45 f. Dissertação (Mestrado em Química) - Universidade Federal de Goiás, Goiânia, 2018.
url http://repositorio.bc.ufg.br/tede/handle/tede/8813
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dc.publisher.none.fl_str_mv Universidade Federal de Goiás
dc.publisher.program.fl_str_mv Programa de Pós-graduação em Química (IQ)
dc.publisher.initials.fl_str_mv UFG
dc.publisher.country.fl_str_mv Brasil
dc.publisher.department.fl_str_mv Instituto de Química - IQ (RG)
publisher.none.fl_str_mv Universidade Federal de Goiás
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repository.name.fl_str_mv Repositório Institucional da UFG - Universidade Federal de Goiás (UFG)
repository.mail.fl_str_mv tasesdissertacoes.bc@ufg.br
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