Métodos para a determinação enantiomérica dos fármacos omeprazol, lansoprazol e pantoprazol em águas residuais e de estuário
Autor(a) principal: | |
---|---|
Data de Publicação: | 2009 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Repositório Institucional da UFSCAR |
Texto Completo: | https://repositorio.ufscar.br/handle/ufscar/6449 |
Resumo: | The use of restricted access media columns for direct injection of samples chemically complex is consolidated, but not for environmental samples. This work describes the conditions for exclusion of aquatic fulvic and humic acids. The analyses were performed comparing the areas obtained after direct injection of standards in a chromatography column of gel permeation (Tsk gel® G3000PWXL), and those obtained in in-line mode with the RAM-BSA. Through a calibration curve, using standards of sodium polystyrene sulfonates of different molecular weights, in order of the 18000 Da, the molecular weight of eluted fractions were determined. This work reports the development, validation and application of sensitive, precise and accuracy methods, by high performance liquid chromatography with direct injection of samples for the enantioselective determination of omeprazole, lansoprazole and pantoprazole drugs in environmental matrices (wastewater from the city of São Carlos, Brazil and estuarine water of the River Douro, Porto-Portugal). The methods were developed by multidimensional liquid chromatography using an octyl restricted access media bovine serum albumin column (RAM-BSA C8) in the first dimension for the exclusion of macromolecules and extraction of drugs. The enantiomeric separation of omeprazole was achieved in the second dimension with a chiral column, amylose tris (3,5-dimetylphenylcarbamate) coated onto APS-Nucleosil support, and the chiral column amylose tris (3,5- dimethoxyphenylcarbamate) coated onto APS-Nucleosil support it was used for simultaneous enantiomeric separation of lansoprazole and pantoprazole. Aliquots of 500μL of the samples were injected directly into the multidimensional chromatographic system with detection for ultraviolet-visible spectroscopy (UV-vis). The quantification limits obtained for the enantiomers of omeprazole were 15μg.L-1, and for the enantiomers of lansoprazole and pantoprazole 5.0 and 7.5μg.L-1, respectively. Lower quantification limits were obtained for the enantiomers of lansoprazole (0,60μg.L-1) and pantoprazole (0,40μg.L-1) by replacement of the UV-vis detector for the mass spectrometer in a multiple reaction monitoring (MRM) mode and increasing the injection volume for 1000μL. |
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Vanzolini, Kenia LourençoCass, Quezia Bezerrahttp://genos.cnpq.br:12010/dwlattes/owa/prc_imp_cv_int?f_cod=K4781559E6http://lattes.cnpq.br/8140494122257511b9ffc67d-1ef9-410a-86cc-1e946921da9e2016-06-02T20:36:22Z2009-11-182016-06-02T20:36:22Z2009-04-17VANZOLINI, Kenia Lourenço. Methods for the enantiomeric determination of omeprazole, lansoprazole and pantoprazole drugs in estuarine and wastewaters. 2009. 160 f. Dissertação (Mestrado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2009.https://repositorio.ufscar.br/handle/ufscar/6449The use of restricted access media columns for direct injection of samples chemically complex is consolidated, but not for environmental samples. This work describes the conditions for exclusion of aquatic fulvic and humic acids. The analyses were performed comparing the areas obtained after direct injection of standards in a chromatography column of gel permeation (Tsk gel® G3000PWXL), and those obtained in in-line mode with the RAM-BSA. Through a calibration curve, using standards of sodium polystyrene sulfonates of different molecular weights, in order of the 18000 Da, the molecular weight of eluted fractions were determined. This work reports the development, validation and application of sensitive, precise and accuracy methods, by high performance liquid chromatography with direct injection of samples for the enantioselective determination of omeprazole, lansoprazole and pantoprazole drugs in environmental matrices (wastewater from the city of São Carlos, Brazil and estuarine water of the River Douro, Porto-Portugal). The methods were developed by multidimensional liquid chromatography using an octyl restricted access media bovine serum albumin column (RAM-BSA C8) in the first dimension for the exclusion of macromolecules and extraction of drugs. The enantiomeric separation of omeprazole was achieved in the second dimension with a chiral column, amylose tris (3,5-dimetylphenylcarbamate) coated onto APS-Nucleosil support, and the chiral column amylose tris (3,5- dimethoxyphenylcarbamate) coated onto APS-Nucleosil support it was used for simultaneous enantiomeric separation of lansoprazole and pantoprazole. Aliquots of 500μL of the samples were injected directly into the multidimensional chromatographic system with detection for ultraviolet-visible spectroscopy (UV-vis). The quantification limits obtained for the enantiomers of omeprazole were 15μg.L-1, and for the enantiomers of lansoprazole and pantoprazole 5.0 and 7.5μg.L-1, respectively. Lower quantification limits were obtained for the enantiomers of lansoprazole (0,60μg.L-1) and pantoprazole (0,40μg.L-1) by replacement of the UV-vis detector for the mass spectrometer in a multiple reaction monitoring (MRM) mode and increasing the injection volume for 1000μL.O uso de colunas de fases de acesso restrito para injeção direta de amostras quimicamente complexas está consolidado, mas não para amostras ambientais. Este trabalho descreve as condições para exclusão de ácidos húmicos e fúlvicos aquáticos. As análises foram feitas comparando as áreas obtidas após injeção direta dos padrões numa coluna cromatográfica de permeação em gel (Tsk gel® G3000PWXL), e as obtidas no modo in-line com as colunas RAM-BSA. Através de uma curva de calibração utilizando padrões de poliestirenos sulfonatos de sódio com diferentes pesos moleculares foi determinado, na ordem de 18000 Da, o peso molecular das frações eluídas. Este trabalho reporta o desenvolvimento, validação e aplicação de métodos sensíveis, precisos e exatos, por cromatografia líquida de alta eficiência com injeção direta de amostras para a determinação enantiosseletiva dos fármacos omeprazol, pantoprazol e lansoprazol, em matrizes ambientais (água residual da cidade de São Carlos-Brasil e água do estuário do Rio Douro, Porto-Portugal). Os métodos foram desenvolvidos por cromatografia liquida multidimensional utilizando-se uma coluna de fase acesso restrito de albumina sérica bovina (RAM-BSA C8), na primeira dimensão, para exclusão das macromoléculas e para extração dos fármacos. A separação enantiomérica do omeprazol foi realizada na segunda dimensão com uma coluna quiral, tris (3,5-dimetilfenilcarbamato) de amilose em APS-Nucleosil e, para os métodos envolvendo a separação enantiomérica simultânea do lansoprazol e pantoprazol foi utilizada a coluna quiral tris (3,5- dimetoxifenilcarbamato) de amilose em APS-Nucleosil. Alíquotas de 500μL das amostras foram injetadas diretamente no sistema cromatográfico multidimensional com detecção por espectroscopia na região do ultravioletaxix visível (UV-vis). Os limites de quantificação obtidos para os enantiômeros do omeprazol foram de 15μg.L-1, e para os enantiômeros do lansoprazol e pantoprazol 5,0 e 7,5μg.L-1, respectivamente. Limites inferiores de quantificação foram obtidos para os enantiômeros do lansoprazol (0,60μg.L-1 ) e pantoprazol (0,40μg.L-1), pela substituição do detector de UV-vis por um espectrômetro de massas, no modo MRM (Multiple Reaction Monitoring), e aumento do volume de injeção para 1000μL.Universidade Federal de Sao Carlosapplication/pdfporUniversidade Federal de São CarlosPrograma de Pós-Graduação em Química - PPGQUFSCarBRCromatografia líquida de alta eficiênciaFármacos quiraisColunas RAMCIENCIAS EXATAS E DA TERRA::QUIMICAMétodos para a determinação enantiomérica dos fármacos omeprazol, lansoprazol e pantoprazol em águas residuais e de estuárioMethods for the enantiomeric determination of omeprazole, lansoprazole and pantoprazole drugs in estuarine and wastewatersinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesis-1-1867fc213-f339-49e1-a669-a1e54cf68bf1info:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFSCARinstname:Universidade Federal de São Carlos (UFSCAR)instacron:UFSCARORIGINAL2537.pdfapplication/pdf7032312https://repositorio.ufscar.br/bitstream/ufscar/6449/1/2537.pdf58b8058ab3f086b95831d5fd832c5897MD51THUMBNAIL2537.pdf.jpg2537.pdf.jpgIM Thumbnailimage/jpeg10743https://repositorio.ufscar.br/bitstream/ufscar/6449/2/2537.pdf.jpg00a964df0989e1d7c4b49b67805dcb9bMD52ufscar/64492023-09-18 18:31:11.407oai:repositorio.ufscar.br:ufscar/6449Repositório InstitucionalPUBhttps://repositorio.ufscar.br/oai/requestopendoar:43222023-09-18T18:31:11Repositório Institucional da UFSCAR - Universidade Federal de São Carlos (UFSCAR)false |
dc.title.por.fl_str_mv |
Métodos para a determinação enantiomérica dos fármacos omeprazol, lansoprazol e pantoprazol em águas residuais e de estuário |
dc.title.alternative.eng.fl_str_mv |
Methods for the enantiomeric determination of omeprazole, lansoprazole and pantoprazole drugs in estuarine and wastewaters |
title |
Métodos para a determinação enantiomérica dos fármacos omeprazol, lansoprazol e pantoprazol em águas residuais e de estuário |
spellingShingle |
Métodos para a determinação enantiomérica dos fármacos omeprazol, lansoprazol e pantoprazol em águas residuais e de estuário Vanzolini, Kenia Lourenço Cromatografia líquida de alta eficiência Fármacos quirais Colunas RAM CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Métodos para a determinação enantiomérica dos fármacos omeprazol, lansoprazol e pantoprazol em águas residuais e de estuário |
title_full |
Métodos para a determinação enantiomérica dos fármacos omeprazol, lansoprazol e pantoprazol em águas residuais e de estuário |
title_fullStr |
Métodos para a determinação enantiomérica dos fármacos omeprazol, lansoprazol e pantoprazol em águas residuais e de estuário |
title_full_unstemmed |
Métodos para a determinação enantiomérica dos fármacos omeprazol, lansoprazol e pantoprazol em águas residuais e de estuário |
title_sort |
Métodos para a determinação enantiomérica dos fármacos omeprazol, lansoprazol e pantoprazol em águas residuais e de estuário |
author |
Vanzolini, Kenia Lourenço |
author_facet |
Vanzolini, Kenia Lourenço |
author_role |
author |
dc.contributor.authorlattes.por.fl_str_mv |
http://lattes.cnpq.br/8140494122257511 |
dc.contributor.author.fl_str_mv |
Vanzolini, Kenia Lourenço |
dc.contributor.advisor1.fl_str_mv |
Cass, Quezia Bezerra |
dc.contributor.advisor1Lattes.fl_str_mv |
http://genos.cnpq.br:12010/dwlattes/owa/prc_imp_cv_int?f_cod=K4781559E6 |
dc.contributor.authorID.fl_str_mv |
b9ffc67d-1ef9-410a-86cc-1e946921da9e |
contributor_str_mv |
Cass, Quezia Bezerra |
dc.subject.por.fl_str_mv |
Cromatografia líquida de alta eficiência Fármacos quirais Colunas RAM |
topic |
Cromatografia líquida de alta eficiência Fármacos quirais Colunas RAM CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.cnpq.fl_str_mv |
CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
The use of restricted access media columns for direct injection of samples chemically complex is consolidated, but not for environmental samples. This work describes the conditions for exclusion of aquatic fulvic and humic acids. The analyses were performed comparing the areas obtained after direct injection of standards in a chromatography column of gel permeation (Tsk gel® G3000PWXL), and those obtained in in-line mode with the RAM-BSA. Through a calibration curve, using standards of sodium polystyrene sulfonates of different molecular weights, in order of the 18000 Da, the molecular weight of eluted fractions were determined. This work reports the development, validation and application of sensitive, precise and accuracy methods, by high performance liquid chromatography with direct injection of samples for the enantioselective determination of omeprazole, lansoprazole and pantoprazole drugs in environmental matrices (wastewater from the city of São Carlos, Brazil and estuarine water of the River Douro, Porto-Portugal). The methods were developed by multidimensional liquid chromatography using an octyl restricted access media bovine serum albumin column (RAM-BSA C8) in the first dimension for the exclusion of macromolecules and extraction of drugs. The enantiomeric separation of omeprazole was achieved in the second dimension with a chiral column, amylose tris (3,5-dimetylphenylcarbamate) coated onto APS-Nucleosil support, and the chiral column amylose tris (3,5- dimethoxyphenylcarbamate) coated onto APS-Nucleosil support it was used for simultaneous enantiomeric separation of lansoprazole and pantoprazole. Aliquots of 500μL of the samples were injected directly into the multidimensional chromatographic system with detection for ultraviolet-visible spectroscopy (UV-vis). The quantification limits obtained for the enantiomers of omeprazole were 15μg.L-1, and for the enantiomers of lansoprazole and pantoprazole 5.0 and 7.5μg.L-1, respectively. Lower quantification limits were obtained for the enantiomers of lansoprazole (0,60μg.L-1) and pantoprazole (0,40μg.L-1) by replacement of the UV-vis detector for the mass spectrometer in a multiple reaction monitoring (MRM) mode and increasing the injection volume for 1000μL. |
publishDate |
2009 |
dc.date.available.fl_str_mv |
2009-11-18 2016-06-02T20:36:22Z |
dc.date.issued.fl_str_mv |
2009-04-17 |
dc.date.accessioned.fl_str_mv |
2016-06-02T20:36:22Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/masterThesis |
format |
masterThesis |
status_str |
publishedVersion |
dc.identifier.citation.fl_str_mv |
VANZOLINI, Kenia Lourenço. Methods for the enantiomeric determination of omeprazole, lansoprazole and pantoprazole drugs in estuarine and wastewaters. 2009. 160 f. Dissertação (Mestrado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2009. |
dc.identifier.uri.fl_str_mv |
https://repositorio.ufscar.br/handle/ufscar/6449 |
identifier_str_mv |
VANZOLINI, Kenia Lourenço. Methods for the enantiomeric determination of omeprazole, lansoprazole and pantoprazole drugs in estuarine and wastewaters. 2009. 160 f. Dissertação (Mestrado em Ciências Exatas e da Terra) - Universidade Federal de São Carlos, São Carlos, 2009. |
url |
https://repositorio.ufscar.br/handle/ufscar/6449 |
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por |
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-1 -1 |
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openAccess |
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Universidade Federal de São Carlos |
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Programa de Pós-Graduação em Química - PPGQ |
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UFSCar |
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BR |
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Universidade Federal de São Carlos |
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