Estudo comparativo entre extração Soxhlet e ultrasom para determinação de hidrocarbonetos policíclicos aromáticos em sedimentos do estuário do rio Sergipe por cromatografia a gás acoplada a espectrometria de massas
Ano de defesa: | 2011 |
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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 Sergipe
|
Programa de Pós-Graduação: |
Pós-Graduação em Química
|
Departamento: |
Não Informado pela instituição
|
País: |
BR
|
Palavras-chave em Português: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | https://ri.ufs.br/handle/riufs/6162 |
Resumo: | Polycyclic aromatic hydrocarbons (PAHs) are compounds that can be found in environmental compartments such as atmosphere, soil, sediment and water. Throughout bioaccumulation, they can also be incorporated into vegetables and animals tissues. They are mainly originated from anthropogenic sources such as fossil fuels and biomass burnings. Due they potential toxicity, carcinogenicity and mutagenicity, they must be carefully monitored. The main goal of this study is to compare two extraction methods (ultrasound and Soxhlet) and the optimization of a cleanup column and chromatographic conditions (GC-MS) for separation and determination of 16 polycyclic aromatic hydrocarbons (PAHs) established as priorities by the Environmental Protection Agency of the United States. Once optimized, the method was applied to evaluate HPAs in sediment samples collected in the Sergipe river estuarine system. The extracts were analyzed by GCMS, using a DB-5 capillary column, splitless injection and operating in SIM mode, with three ions being monitored for each PAH, one ion principal and two others as confirmation ions. We conducted a validation study of the methods. The analytical curves showed coefficients of determination (R2) above 0.99 for all 16 PAHs. For the ultrasound method, the average recovery obtained in two fortification levels (12.5 ng g-1 and 62.5 ng g-1) showed no significant differences, with a recovering average ranging from 74 to 125.4% and RSD <19.2% for all compounds analyzed, except for pyrene. The limits of detection and quantification by ultrasound ranged from 0.04 to 0.23 ng g-1 and 0.12 to 0.78 ng g-1, respectively, and the limits of detection and quantification by Soxhlet ranged from 0.03 to 0.3 ng g-1 and 0.11 to 1.0 ng g-1, respectively. On the other hand, the Soxhlet extraction did not show good recoveries for low molecular weight PAHs, especially naphthalene, acenaphthylene and acenaphthene, with values ranging from 9.5 to 98.4%. Therefore, the extraction method chosen for the analysis of PAHs in sediment was the ultrasound. It showed good recovery, speed, solvent and adsorbent economy and low extraction time. It also allows simultaneous extraction of several samples. The total concentrations of PAHs in the sediments studied ranged from 6.7 ng g-1 to 377.7 ng g-1 dry weight. The species found in higher concentrations were Benzo[ghi]Perylene (61.9 ng g-1), chrysene (52.7 ng g- 1), fluoranthene (47.9 ng g-1) and pyrene (34.1 ng g-1). The investigation of the PAHs sources suggests pyrogenic origin for most of the compounds. |
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Santos, Antonio Sérgio Oliveira doshttp://lattes.cnpq.br/3464513435840165Dórea, Haroldo Silveirahttp://lattes.cnpq.br/90445376121960902017-09-27T13:58:14Z2017-09-27T13:58:14Z2011-08-26https://ri.ufs.br/handle/riufs/6162Polycyclic aromatic hydrocarbons (PAHs) are compounds that can be found in environmental compartments such as atmosphere, soil, sediment and water. Throughout bioaccumulation, they can also be incorporated into vegetables and animals tissues. They are mainly originated from anthropogenic sources such as fossil fuels and biomass burnings. Due they potential toxicity, carcinogenicity and mutagenicity, they must be carefully monitored. The main goal of this study is to compare two extraction methods (ultrasound and Soxhlet) and the optimization of a cleanup column and chromatographic conditions (GC-MS) for separation and determination of 16 polycyclic aromatic hydrocarbons (PAHs) established as priorities by the Environmental Protection Agency of the United States. Once optimized, the method was applied to evaluate HPAs in sediment samples collected in the Sergipe river estuarine system. The extracts were analyzed by GCMS, using a DB-5 capillary column, splitless injection and operating in SIM mode, with three ions being monitored for each PAH, one ion principal and two others as confirmation ions. We conducted a validation study of the methods. The analytical curves showed coefficients of determination (R2) above 0.99 for all 16 PAHs. For the ultrasound method, the average recovery obtained in two fortification levels (12.5 ng g-1 and 62.5 ng g-1) showed no significant differences, with a recovering average ranging from 74 to 125.4% and RSD <19.2% for all compounds analyzed, except for pyrene. The limits of detection and quantification by ultrasound ranged from 0.04 to 0.23 ng g-1 and 0.12 to 0.78 ng g-1, respectively, and the limits of detection and quantification by Soxhlet ranged from 0.03 to 0.3 ng g-1 and 0.11 to 1.0 ng g-1, respectively. On the other hand, the Soxhlet extraction did not show good recoveries for low molecular weight PAHs, especially naphthalene, acenaphthylene and acenaphthene, with values ranging from 9.5 to 98.4%. Therefore, the extraction method chosen for the analysis of PAHs in sediment was the ultrasound. It showed good recovery, speed, solvent and adsorbent economy and low extraction time. It also allows simultaneous extraction of several samples. The total concentrations of PAHs in the sediments studied ranged from 6.7 ng g-1 to 377.7 ng g-1 dry weight. The species found in higher concentrations were Benzo[ghi]Perylene (61.9 ng g-1), chrysene (52.7 ng g- 1), fluoranthene (47.9 ng g-1) and pyrene (34.1 ng g-1). The investigation of the PAHs sources suggests pyrogenic origin for most of the compounds.Os hidrocarbonetos policíclicos aromáticos (HPAs) são compostos que podem ser encontrados em diversos compartimentos ambientais tais como atmosfera, solo, sedimento e água. Por bioacumulação podem também estar incorporados aos organismos vegetais e animais. São originados, principalmente, de fontes e/ou atividades antrópicas, como a queima de combustíveis fósseis e da biomassa. Devido ao seu potencial tóxico, carcinogênico e mutagênico, eles devem ser cuidadosamente monitorados. O presente trabalho tem como objetivo a comparação de dois métodos de extração (ultra-som e Soxhlet), otimização de uma coluna (clean up) e das condições cromatográficas (GC-MS) para a separação e determinação dos 16 hidrocarbonetos policíclicos aromáticos (HPAs), estabelecidos como prioritários pela Agência de Proteção Ambiental dos Estados Unidos, em amostras de sedimentos coletadas no estuário do rio Sergipe. Os extratos foram analisados por GC-MS utilizando coluna capilar DB-5, injeção no modo splitless e operando no modo SIM, selecionando um íon principal e dois de confirmação de cada HPA. Foi realizado um estudo de validação dos métodos. As curvas analíticas apresentaram valores de coeficiente de determinação (R2) acima de 0,99 para os 16 HPAs. Pelo método de ultra-som, os valores médios de recuperação obtidos em dois níveis de fortificação (12,5 ng g-1 e 62,5 ng g-1) não apresentaram diferenças significativas, obtendo recuperação média na faixa de 74 a 125,4% e RSD< 19,2% para os compostos analisados, com exceção do pireno. Os limites de detecção e quantificação por ultra-som variaram de 0,04 a 0,23 ng g-1 e de 0,12 a 0,78 ng g-1, respectivamente, enquanto que por Soxhlet variaram de 0,03 a 0,3 ng g-1 e de 0,11 a 1,0 ng g-1, respectivamente. Por outro lado, a extração por Soxhlet não apresentou boa recuperação para os HPAs de baixa massa molar, principalmente, o naftaleno, acenaftileno e o acenafteno, que variou de 9,5 a 98,4%. Portanto, o procedimento escolhido para análise de HPAs em sedimento foi o ultra-som, pois mostrou boa recuperação, rapidez, economia de solvente e adsorvente, baixo tempo de extração, além de permitir a extração simultânea de todas as amostras. As concentrações de HPAs totais nos sedimentos estudados variaram de 6,7 ng g-1 a 377,7 ng g-1 em peso seco. As espécies encontradas em maior concentração foram Benzo[ghi]Perileno (61,9 ng g-1), Criseno (52,7 ng g-1), Fluoranteno (47,9 ng g-1) e Pireno (34,1 ng g-1). A investigação da fonte dos HPAs sugere origem pirogênica para a maioria dos compostos.application/pdfporUniversidade Federal de SergipePós-Graduação em QuímicaUFSBRHPAsGC/MSSoxhletUltra-somSedimentoRio SergipePAHsGC / MSSoxhletUltrasoundSedimentSergipe riverCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAEstudo comparativo entre extração Soxhlet e ultrasom para determinação de hidrocarbonetos policíclicos aromáticos em sedimentos do estuário do rio Sergipe por cromatografia a gás acoplada a espectrometria de massasCOMPARATIVE STUDY OF EXTRACTION SOXHLET AND ULTRASOUND DETERMINATION FOR OIL POLYCYCLIC AROMATIC SEDIMENTS SERGIPE RIVER ESTUARY BY GAS CHROMATOGRAPHY MASS SPECTROMETRY ATTACHED.info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisinfo:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFSinstname:Universidade Federal de Sergipe (UFS)instacron:UFSORIGINALANTONIO_SERGIO_OLIVEIRA_SANTOS.pdfapplication/pdf1595658https://ri.ufs.br/jspui/bitstream/riufs/6162/1/ANTONIO_SERGIO_OLIVEIRA_SANTOS.pdf6bb937282b93d8b1a111d76bc824b563MD51TEXTANTONIO_SERGIO_OLIVEIRA_SANTOS.pdf.txtANTONIO_SERGIO_OLIVEIRA_SANTOS.pdf.txtExtracted texttext/plain143833https://ri.ufs.br/jspui/bitstream/riufs/6162/2/ANTONIO_SERGIO_OLIVEIRA_SANTOS.pdf.txt540e6784ae28cf15e6a9aa51dc37711cMD52THUMBNAILANTONIO_SERGIO_OLIVEIRA_SANTOS.pdf.jpgANTONIO_SERGIO_OLIVEIRA_SANTOS.pdf.jpgGenerated Thumbnailimage/jpeg1434https://ri.ufs.br/jspui/bitstream/riufs/6162/3/ANTONIO_SERGIO_OLIVEIRA_SANTOS.pdf.jpg73e51d8abcdd69205c495b54ff83894dMD53riufs/61622018-01-16 19:40:38.72oai:ufs.br:riufs/6162Repositório InstitucionalPUBhttps://ri.ufs.br/oai/requestrepositorio@academico.ufs.bropendoar:2018-01-16T22:40:38Repositório Institucional da UFS - Universidade Federal de Sergipe (UFS)false |
dc.title.por.fl_str_mv |
Estudo comparativo entre extração Soxhlet e ultrasom para determinação de hidrocarbonetos policíclicos aromáticos em sedimentos do estuário do rio Sergipe por cromatografia a gás acoplada a espectrometria de massas |
dc.title.alternative.eng.fl_str_mv |
COMPARATIVE STUDY OF EXTRACTION SOXHLET AND ULTRASOUND DETERMINATION FOR OIL POLYCYCLIC AROMATIC SEDIMENTS SERGIPE RIVER ESTUARY BY GAS CHROMATOGRAPHY MASS SPECTROMETRY ATTACHED. |
title |
Estudo comparativo entre extração Soxhlet e ultrasom para determinação de hidrocarbonetos policíclicos aromáticos em sedimentos do estuário do rio Sergipe por cromatografia a gás acoplada a espectrometria de massas |
spellingShingle |
Estudo comparativo entre extração Soxhlet e ultrasom para determinação de hidrocarbonetos policíclicos aromáticos em sedimentos do estuário do rio Sergipe por cromatografia a gás acoplada a espectrometria de massas Santos, Antonio Sérgio Oliveira dos HPAs GC/MS Soxhlet Ultra-som Sedimento Rio Sergipe PAHs GC / MS Soxhlet Ultrasound Sediment Sergipe river CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Estudo comparativo entre extração Soxhlet e ultrasom para determinação de hidrocarbonetos policíclicos aromáticos em sedimentos do estuário do rio Sergipe por cromatografia a gás acoplada a espectrometria de massas |
title_full |
Estudo comparativo entre extração Soxhlet e ultrasom para determinação de hidrocarbonetos policíclicos aromáticos em sedimentos do estuário do rio Sergipe por cromatografia a gás acoplada a espectrometria de massas |
title_fullStr |
Estudo comparativo entre extração Soxhlet e ultrasom para determinação de hidrocarbonetos policíclicos aromáticos em sedimentos do estuário do rio Sergipe por cromatografia a gás acoplada a espectrometria de massas |
title_full_unstemmed |
Estudo comparativo entre extração Soxhlet e ultrasom para determinação de hidrocarbonetos policíclicos aromáticos em sedimentos do estuário do rio Sergipe por cromatografia a gás acoplada a espectrometria de massas |
title_sort |
Estudo comparativo entre extração Soxhlet e ultrasom para determinação de hidrocarbonetos policíclicos aromáticos em sedimentos do estuário do rio Sergipe por cromatografia a gás acoplada a espectrometria de massas |
author |
Santos, Antonio Sérgio Oliveira dos |
author_facet |
Santos, Antonio Sérgio Oliveira dos |
author_role |
author |
dc.contributor.author.fl_str_mv |
Santos, Antonio Sérgio Oliveira dos |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/3464513435840165 |
dc.contributor.advisor1.fl_str_mv |
Dórea, Haroldo Silveira |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/9044537612196090 |
contributor_str_mv |
Dórea, Haroldo Silveira |
dc.subject.por.fl_str_mv |
HPAs GC/MS Soxhlet Ultra-som Sedimento Rio Sergipe |
topic |
HPAs GC/MS Soxhlet Ultra-som Sedimento Rio Sergipe PAHs GC / MS Soxhlet Ultrasound Sediment Sergipe river CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
PAHs GC / MS Soxhlet Ultrasound Sediment Sergipe river |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
Polycyclic aromatic hydrocarbons (PAHs) are compounds that can be found in environmental compartments such as atmosphere, soil, sediment and water. Throughout bioaccumulation, they can also be incorporated into vegetables and animals tissues. They are mainly originated from anthropogenic sources such as fossil fuels and biomass burnings. Due they potential toxicity, carcinogenicity and mutagenicity, they must be carefully monitored. The main goal of this study is to compare two extraction methods (ultrasound and Soxhlet) and the optimization of a cleanup column and chromatographic conditions (GC-MS) for separation and determination of 16 polycyclic aromatic hydrocarbons (PAHs) established as priorities by the Environmental Protection Agency of the United States. Once optimized, the method was applied to evaluate HPAs in sediment samples collected in the Sergipe river estuarine system. The extracts were analyzed by GCMS, using a DB-5 capillary column, splitless injection and operating in SIM mode, with three ions being monitored for each PAH, one ion principal and two others as confirmation ions. We conducted a validation study of the methods. The analytical curves showed coefficients of determination (R2) above 0.99 for all 16 PAHs. For the ultrasound method, the average recovery obtained in two fortification levels (12.5 ng g-1 and 62.5 ng g-1) showed no significant differences, with a recovering average ranging from 74 to 125.4% and RSD <19.2% for all compounds analyzed, except for pyrene. The limits of detection and quantification by ultrasound ranged from 0.04 to 0.23 ng g-1 and 0.12 to 0.78 ng g-1, respectively, and the limits of detection and quantification by Soxhlet ranged from 0.03 to 0.3 ng g-1 and 0.11 to 1.0 ng g-1, respectively. On the other hand, the Soxhlet extraction did not show good recoveries for low molecular weight PAHs, especially naphthalene, acenaphthylene and acenaphthene, with values ranging from 9.5 to 98.4%. Therefore, the extraction method chosen for the analysis of PAHs in sediment was the ultrasound. It showed good recovery, speed, solvent and adsorbent economy and low extraction time. It also allows simultaneous extraction of several samples. The total concentrations of PAHs in the sediments studied ranged from 6.7 ng g-1 to 377.7 ng g-1 dry weight. The species found in higher concentrations were Benzo[ghi]Perylene (61.9 ng g-1), chrysene (52.7 ng g- 1), fluoranthene (47.9 ng g-1) and pyrene (34.1 ng g-1). The investigation of the PAHs sources suggests pyrogenic origin for most of the compounds. |
publishDate |
2011 |
dc.date.issued.fl_str_mv |
2011-08-26 |
dc.date.accessioned.fl_str_mv |
2017-09-27T13:58:14Z |
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2017-09-27T13:58:14Z |
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Universidade Federal de Sergipe |
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