Investigação da adequabilidade da cromatografia de íons para a determinação de espécies de halogênios em saliva
Autor(a) principal: | |
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Data de Publicação: | 2019 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Manancial - Repositório Digital da UFSM |
Texto Completo: | http://repositorio.ufsm.br/handle/1/20632 |
Resumo: | In this work, ion chromatography was investigated for halogens speciation analysis in human saliva. Initially, it was used an isocratic ion chromatography system (“IC 1 System”), being evaluated: the chromatographic column (Metrosep A Supp 7 or Metrosep A Supp 5), the composition of the mobile phase (Na2CO3 or Na2CO3 + NaHCO3), the mobile phase flow rate (between 0.4 to 0.8 mL min-1, depending on the column), the temperature of the column compartment (30 to 45 °C), and the use of mobile phase modifiers (acetone). A system that allows operating in gradient mode (“IC 2 System”) was also evaluated, being optimized: the temperature of the column compartment (20 to 45 °C), the eluent flow rate (0.15 to 0.40 mL min-1) and different gradient programs (1 to 60 mmol L-1 KOH). Microwave-assisted alkaline dissolution was used to obtain the total halogen concentration by inductively coupled plasma mass spectrometry (ICP-MS). The best condition found for the “IC 1 System” was obtained with the Metrosep A Supp 7 column at 45 °C using Na2CO3 (3.6 mmol L-1) as the mobile phase, at 0.8 mL min-1. However, this condition did not provide the separation of fluoride and iodate and also, bromide, chlorate and perchlorate. The “IC 2 System” enabled the separation of bromide from chlorate and perchlorate according to the gradient elution program. The optimized conditions for the “IC 2 System” were 1 to 60 mmol L-1 KOH gradient, 0.3 mL min-1 mobile phase flow rate and column compartment temperature at 35 °C. In addition to chromatographic evaluations, the stability of halogens in saliva was also studied, as well as the use of different filtration membranes for sample pretreatment. The stability study demonstrated the viability of storage for up to 90 days under refrigeration (4 °C), without leading to losses in total Cl, Br and I concentration. Regarding the use of a filtration step as pretreatment, different membrane types were investigated and no influence was observed for Cl and Br. However, Cl contamination was observed in some filters and underestimated results were observed for iodine. Additionally, the IC systems presented wide linear range (5-10000 μg L-1), as well as low limits of detection and quantification for the investigated species. With the developed method, it was possible to identify chloride and bromide, as well as sulfate and phosphate in human saliva. |
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Investigação da adequabilidade da cromatografia de íons para a determinação de espécies de halogênios em salivaInvestigation of the adequability of ion chromatography for halogens speciation analysis in salivaAnálise de especiaçãoHalogêniosCromatografia de íonsSalivaEstabilidadeSpeciation analysisHalogensIon chromatographySalivaStabilityCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAIn this work, ion chromatography was investigated for halogens speciation analysis in human saliva. Initially, it was used an isocratic ion chromatography system (“IC 1 System”), being evaluated: the chromatographic column (Metrosep A Supp 7 or Metrosep A Supp 5), the composition of the mobile phase (Na2CO3 or Na2CO3 + NaHCO3), the mobile phase flow rate (between 0.4 to 0.8 mL min-1, depending on the column), the temperature of the column compartment (30 to 45 °C), and the use of mobile phase modifiers (acetone). A system that allows operating in gradient mode (“IC 2 System”) was also evaluated, being optimized: the temperature of the column compartment (20 to 45 °C), the eluent flow rate (0.15 to 0.40 mL min-1) and different gradient programs (1 to 60 mmol L-1 KOH). Microwave-assisted alkaline dissolution was used to obtain the total halogen concentration by inductively coupled plasma mass spectrometry (ICP-MS). The best condition found for the “IC 1 System” was obtained with the Metrosep A Supp 7 column at 45 °C using Na2CO3 (3.6 mmol L-1) as the mobile phase, at 0.8 mL min-1. However, this condition did not provide the separation of fluoride and iodate and also, bromide, chlorate and perchlorate. The “IC 2 System” enabled the separation of bromide from chlorate and perchlorate according to the gradient elution program. The optimized conditions for the “IC 2 System” were 1 to 60 mmol L-1 KOH gradient, 0.3 mL min-1 mobile phase flow rate and column compartment temperature at 35 °C. In addition to chromatographic evaluations, the stability of halogens in saliva was also studied, as well as the use of different filtration membranes for sample pretreatment. The stability study demonstrated the viability of storage for up to 90 days under refrigeration (4 °C), without leading to losses in total Cl, Br and I concentration. Regarding the use of a filtration step as pretreatment, different membrane types were investigated and no influence was observed for Cl and Br. However, Cl contamination was observed in some filters and underestimated results were observed for iodine. Additionally, the IC systems presented wide linear range (5-10000 μg L-1), as well as low limits of detection and quantification for the investigated species. With the developed method, it was possible to identify chloride and bromide, as well as sulfate and phosphate in human saliva.Conselho Nacional de Pesquisa e Desenvolvimento Científico e Tecnológico - CNPqNeste trabalho, a cromatografia de troca iônica foi investigada para análise de especiação de halogênios em saliva humana. Inicialmente, foi utilizado um sistema de cromatografia de íons que opera no modo isocrático (“Sistema IC 1”), sendo avaliados: a coluna cromatográfica (Metrosep A Supp 7 ou Metrosep A Supp 5), a composição da fase móvel (Na2CO3 e Na2CO3 + NaHCO3), a vazão da fase móvel (entre 0,4 a 0,8 mL min-1, dependendo da coluna), a temperatura do compartimento da coluna (30 a 45 °C), e, ainda, o uso de modificador na fase móvel (acetona). Na sequência foi avaliado um sistema que permite operar no modo gradiente (“Sistema IC 2”), sendo otimizados: a temperatura do compartimento da coluna (20 a 45 °C), a vazão do eluente (0,15 a 0,40 mL min-1) e diferentes programas de eluição por gradiente (1 a 60 mmol L-1 de KOH). A dissolução alcalina assistida por micro-ondas foi utilizada para obter a concentração de halogênios total por espectrometria de massa com plasma indutivamente acoplado (ICP-MS). A melhor condição obtida com o “Sistema IC 1” foi obtida com a coluna Metrosep A Supp 7, a 45 °C, utilizando Na2CO3 (3,6 mmol L-1) como fase móvel, a 0,8 mL min-1. Contudo, esta condição não proporcionou a separação entre fluoreto e iodato e, entre brometo, clorato e perclorato. O “Sistema IC 2”, possibilitou a separação de brometo do par cloratoperclorato devido ao programa de eluição por gradiente. Com o “Sistema IC 2”, a melhor condição de separação foi obtida com eluição por gradiente de 1 a 60 mmol L-1 de KOH, vazão de fase móvel de 0,3 mL min-1 e temperatura do compartimento da coluna em 35 °C. Além das avaliações cromatográficas, foi avaliada também a estabilidade dos halogênios na saliva, bem como o uso de diferentes membranas de filtração para o pré-tratamento da amostra. O estudo de estabilidade demonstrou a viabilidade de armazenamento por até 90 dias, quando a amostra é armazenada sob refrigeração (4 °C), sem representar perdas na concentração de Cl, Br e I total. Quanto ao uso de uma etapa de filtração como pré-tratamento, foram investigados diferentes tipos de membrana e não foi observada influência para Cl e Br. Contudo, foi observada contaminação para Cl em alguns filtros e resultados subestimados foram observados para iodo. Adicionalmente, os sistemas de IC apresentaram ampla faixa linear (5-10000 μg L-1), bem como baixos limites de detecção e de quantificação para as espécies investigadas. Com o método desenvolvido, foi possível identificar cloreto e brometo, além de sulfato e fosfato em saliva humana.Universidade Federal de Santa MariaBrasilQuímicaUFSMPrograma de Pós-Graduação em QuímicaCentro de Ciências Naturais e ExatasMello, Paola de Azevedohttp://lattes.cnpq.br/2189500441942469Mesko, Márcia FosterXXXXXXXXXXXXXXXBolzan, Rodrigo CordeiroXXXXXXXXXXXXXXMendes, Ana Luiza Garcia2021-04-20T09:40:56Z2021-04-20T09:40:56Z2019-08-15info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisapplication/pdfhttp://repositorio.ufsm.br/handle/1/20632porAttribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/info:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSM2021-04-21T06:02:38Zoai:repositorio.ufsm.br:1/20632Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2021-04-21T06:02:38Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.none.fl_str_mv |
Investigação da adequabilidade da cromatografia de íons para a determinação de espécies de halogênios em saliva Investigation of the adequability of ion chromatography for halogens speciation analysis in saliva |
title |
Investigação da adequabilidade da cromatografia de íons para a determinação de espécies de halogênios em saliva |
spellingShingle |
Investigação da adequabilidade da cromatografia de íons para a determinação de espécies de halogênios em saliva Mendes, Ana Luiza Garcia Análise de especiação Halogênios Cromatografia de íons Saliva Estabilidade Speciation analysis Halogens Ion chromatography Saliva Stability CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Investigação da adequabilidade da cromatografia de íons para a determinação de espécies de halogênios em saliva |
title_full |
Investigação da adequabilidade da cromatografia de íons para a determinação de espécies de halogênios em saliva |
title_fullStr |
Investigação da adequabilidade da cromatografia de íons para a determinação de espécies de halogênios em saliva |
title_full_unstemmed |
Investigação da adequabilidade da cromatografia de íons para a determinação de espécies de halogênios em saliva |
title_sort |
Investigação da adequabilidade da cromatografia de íons para a determinação de espécies de halogênios em saliva |
author |
Mendes, Ana Luiza Garcia |
author_facet |
Mendes, Ana Luiza Garcia |
author_role |
author |
dc.contributor.none.fl_str_mv |
Mello, Paola de Azevedo http://lattes.cnpq.br/2189500441942469 Mesko, Márcia Foster XXXXXXXXXXXXXXX Bolzan, Rodrigo Cordeiro XXXXXXXXXXXXXX |
dc.contributor.author.fl_str_mv |
Mendes, Ana Luiza Garcia |
dc.subject.por.fl_str_mv |
Análise de especiação Halogênios Cromatografia de íons Saliva Estabilidade Speciation analysis Halogens Ion chromatography Saliva Stability CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
topic |
Análise de especiação Halogênios Cromatografia de íons Saliva Estabilidade Speciation analysis Halogens Ion chromatography Saliva Stability CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this work, ion chromatography was investigated for halogens speciation analysis in human saliva. Initially, it was used an isocratic ion chromatography system (“IC 1 System”), being evaluated: the chromatographic column (Metrosep A Supp 7 or Metrosep A Supp 5), the composition of the mobile phase (Na2CO3 or Na2CO3 + NaHCO3), the mobile phase flow rate (between 0.4 to 0.8 mL min-1, depending on the column), the temperature of the column compartment (30 to 45 °C), and the use of mobile phase modifiers (acetone). A system that allows operating in gradient mode (“IC 2 System”) was also evaluated, being optimized: the temperature of the column compartment (20 to 45 °C), the eluent flow rate (0.15 to 0.40 mL min-1) and different gradient programs (1 to 60 mmol L-1 KOH). Microwave-assisted alkaline dissolution was used to obtain the total halogen concentration by inductively coupled plasma mass spectrometry (ICP-MS). The best condition found for the “IC 1 System” was obtained with the Metrosep A Supp 7 column at 45 °C using Na2CO3 (3.6 mmol L-1) as the mobile phase, at 0.8 mL min-1. However, this condition did not provide the separation of fluoride and iodate and also, bromide, chlorate and perchlorate. The “IC 2 System” enabled the separation of bromide from chlorate and perchlorate according to the gradient elution program. The optimized conditions for the “IC 2 System” were 1 to 60 mmol L-1 KOH gradient, 0.3 mL min-1 mobile phase flow rate and column compartment temperature at 35 °C. In addition to chromatographic evaluations, the stability of halogens in saliva was also studied, as well as the use of different filtration membranes for sample pretreatment. The stability study demonstrated the viability of storage for up to 90 days under refrigeration (4 °C), without leading to losses in total Cl, Br and I concentration. Regarding the use of a filtration step as pretreatment, different membrane types were investigated and no influence was observed for Cl and Br. However, Cl contamination was observed in some filters and underestimated results were observed for iodine. Additionally, the IC systems presented wide linear range (5-10000 μg L-1), as well as low limits of detection and quantification for the investigated species. With the developed method, it was possible to identify chloride and bromide, as well as sulfate and phosphate in human saliva. |
publishDate |
2019 |
dc.date.none.fl_str_mv |
2019-08-15 2021-04-20T09:40:56Z 2021-04-20T09:40:56Z |
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.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/20632 |
url |
http://repositorio.ufsm.br/handle/1/20632 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.rights.driver.fl_str_mv |
Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ info:eu-repo/semantics/openAccess |
rights_invalid_str_mv |
Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ |
eu_rights_str_mv |
openAccess |
dc.format.none.fl_str_mv |
application/pdf |
dc.publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Brasil Química UFSM Programa de Pós-Graduação em Química Centro de Ciências Naturais e Exatas |
publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Brasil Química UFSM Programa de Pós-Graduação em Química Centro de Ciências Naturais e Exatas |
dc.source.none.fl_str_mv |
reponame:Manancial - Repositório Digital da UFSM instname:Universidade Federal de Santa Maria (UFSM) instacron:UFSM |
instname_str |
Universidade Federal de Santa Maria (UFSM) |
instacron_str |
UFSM |
institution |
UFSM |
reponame_str |
Manancial - Repositório Digital da UFSM |
collection |
Manancial - Repositório Digital da UFSM |
repository.name.fl_str_mv |
Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
atendimento.sib@ufsm.br||tedebc@gmail.com |
_version_ |
1805922118848741376 |