Espécies de arsênio em moluscos bivalves determinadas por LC-ICP-MS E LC-CVG-ICP-MS após extração assistida por microondas
Autor(a) principal: | |
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Data de Publicação: | 2013 |
Tipo de documento: | Tese |
Idioma: | por |
Título da fonte: | Biblioteca Digital de Teses e Dissertações do UFSM |
Texto Completo: | http://repositorio.ufsm.br/handle/1/4249 |
Resumo: | In this work, the aim of this study is to evaluate sample preparation procedures and liquid chromatography-inductively coupled plasma mass spectrometry (LC-ICP-MS) and LC coupled to chemical vapor generation (CVG) and ICP-MS (LC-CVG-ICP-MS) for identification and quantification of As species in mollusks collected in BTS. Conditions related to As species extraction were assessed with the use of microwave assisted extraction (MAE) and ultrasound-assisted extraction (UAE). The influence of the main parameters involved in extraction of As species such as the type and concentration of extraction solution, sample mass, temperature and extraction time were evaluated. The extraction was possible by using water at 80 °C (0.2 g sample and 6 mL of w ater) for 6 min using MAE. For the chromatographic separation the type of mobile phase [(NH4)2CO3 and (NH4)2HPO4] concentration (1 to 20 mmol L-1), pH (5.0 to 9.0), flow rate (1.05 to 1.45 mL min-1) and elution mode (isocratic and gradient) were evaluated. The volume of sample injected into the chromatograph was fixed to 200 μL. For the separation of As species an anion exchange column (Hamilton PRP-X100, 250 x 4.1 mm) was used. Six As species were detected in the mollusks being identified arsenobetaine (AsB), As(III), dimethylarsenic acid (DMA) and ρ- arsanilic acid (ρ-ASA). The best separation of the As species was obtained by gradient elution mode and using the following program: 0 to 1.4 min using 6 mmol L-1 (NH4)2HPO4 to 1.4 to 2.7 min using 20 mmol L-1 (NH4)2CO3 and 2.7 to 15 min using 6 mmol L-1 (NH4)2HPO4). The mobile phase flow rate was set at 1.25 mL min-1. CVG parameters were evaluated and the concentrations of NaBH4 and HCl, and carrier gas flow rate were set to 1.0% (m/v) 1.0 mol L-1 and 1.15 L min-1, respectively. The extraction procedures and determination of total As were evaluated using certified reference materials BCR 627 (Tuna Fish Tissue), DORM-2 (Dogfish Muscle) and NIST 1566b (Oyster tissue). The agreement of the results obtained was 95 ± 3 to 101 ± 5%, respectively. The sum of the concentrations of As species determined by LC-ICP-MS and the total As concentration in digested samples and extracts measured, determined by ICP OES were also in good agreement on a confidence level of 95% (Student t-Test). The developed methods by employing the LC-ICP-MS and LC-CVGICP- MS for As speciation analyses in bivalves mollusks are considered suitable. |
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2017-05-112017-05-112013-03-05SANTOS, Clarissa Marques Moreira dos. Espécies de arsênio em moluscos bivalves determinadas por LC-ICP-MS E LC-CVG-ICP-MS após extração assistida por microondas. 2013. 155 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013.http://repositorio.ufsm.br/handle/1/4249In this work, the aim of this study is to evaluate sample preparation procedures and liquid chromatography-inductively coupled plasma mass spectrometry (LC-ICP-MS) and LC coupled to chemical vapor generation (CVG) and ICP-MS (LC-CVG-ICP-MS) for identification and quantification of As species in mollusks collected in BTS. Conditions related to As species extraction were assessed with the use of microwave assisted extraction (MAE) and ultrasound-assisted extraction (UAE). The influence of the main parameters involved in extraction of As species such as the type and concentration of extraction solution, sample mass, temperature and extraction time were evaluated. The extraction was possible by using water at 80 °C (0.2 g sample and 6 mL of w ater) for 6 min using MAE. For the chromatographic separation the type of mobile phase [(NH4)2CO3 and (NH4)2HPO4] concentration (1 to 20 mmol L-1), pH (5.0 to 9.0), flow rate (1.05 to 1.45 mL min-1) and elution mode (isocratic and gradient) were evaluated. The volume of sample injected into the chromatograph was fixed to 200 μL. For the separation of As species an anion exchange column (Hamilton PRP-X100, 250 x 4.1 mm) was used. Six As species were detected in the mollusks being identified arsenobetaine (AsB), As(III), dimethylarsenic acid (DMA) and ρ- arsanilic acid (ρ-ASA). The best separation of the As species was obtained by gradient elution mode and using the following program: 0 to 1.4 min using 6 mmol L-1 (NH4)2HPO4 to 1.4 to 2.7 min using 20 mmol L-1 (NH4)2CO3 and 2.7 to 15 min using 6 mmol L-1 (NH4)2HPO4). The mobile phase flow rate was set at 1.25 mL min-1. CVG parameters were evaluated and the concentrations of NaBH4 and HCl, and carrier gas flow rate were set to 1.0% (m/v) 1.0 mol L-1 and 1.15 L min-1, respectively. The extraction procedures and determination of total As were evaluated using certified reference materials BCR 627 (Tuna Fish Tissue), DORM-2 (Dogfish Muscle) and NIST 1566b (Oyster tissue). The agreement of the results obtained was 95 ± 3 to 101 ± 5%, respectively. The sum of the concentrations of As species determined by LC-ICP-MS and the total As concentration in digested samples and extracts measured, determined by ICP OES were also in good agreement on a confidence level of 95% (Student t-Test). The developed methods by employing the LC-ICP-MS and LC-CVGICP- MS for As speciation analyses in bivalves mollusks are considered suitable.Neste trabalho foi avaliado o preparo da amostra e o uso da cromatografia a líquido acoplada à espectrometria de massa com plasma indutivamente acoplado (LC-ICP-MS) e LC acoplado ao sistema de geração química de vapor (CVG) e ICP-MS para a identificação e quantificação das espécies de As presentes em tecidos de moluscos bivalves. Condições relacionadas à extração das espécies de As foram avaliadas com o emprego de extração assistida por micro-ondas (MAE) e ultrassom (UAE). A influência dos principais parâmetros envolvidos na extração das espécies de As, como o tipo e concentração da solução extratora, massa de amostra, temperatura e o tempo de extração por MAE e o tempo de sonicação por US foram avaliados. Extração de As foi possível usando água a 80 °C (0,2 g de amostra e 6 mL de água) durante 6 min com MAE. Para a separação cromatográfica foram avaliados o tipo de fase móvel [(NH4)2CO3 e (NH4)2HPO4], a concentração (1 a 20 mmol L-1), o pH (5,0 a 9,0), a vazão (1,05 a 1,45 mL min-1) e o modo de eluição (isocrático e gradiente). O volume de amostra injetada no cromatógrafo foi fixado em 200 μL. Para a separação das espécies de As foi utilizada uma coluna de troca aniônica (Hamilton PRPX100, 250 x 4,1 mm). Foram detectadas seis espécies de As nos moluscos, sendo identificadas somente a arsenobetaína (AsB), o As(III), o dimetilarsênio (DMA) e o ácido ρ- arsanílico (ρ-ASA). A melhor separação das espécies de As foi obtida por eluição gradiente utilizando as seguintes condições: 0 a 1,4 min empregando 6 mmol L-1 de (NH4)2HPO4, 1,4 a 2,7 min empregando 20 mmol L-1 de (NH4)2CO3 e 2,7 a 15 min utilizando 6 mmol L-1 de (NH4)2HPO4. A vazão da fase móvel foi fixada em 1,25 mL min-1. Os parâmetros de CVG avaliados foram a concentração de NaBH4 e HCl e a vazão do gás de arraste, as quais foram fixadas em 1,0 % (m/v), 1,0 mol L-1 e 1,15 L min-1, respectivamente. Os procedimentos de extração e determinação de As total foram avaliados utilizando os materiais de referência certificados BCR 627 (Tuna Fish Tissue), DORM-2 (Dogfish Muscle) e NIST 1566b (Oyster tissue). A concordância entre os resultados obtidos foi de 95 ± 3 a 101 ± 5%, respectivamente. Os valores entre a soma das concentrações das espécies de As obtidos por LC-ICP-MS e As total nos digeridos e extratos obtidos, determinado por ICP OES também foram concordantes em um nível de confiança de 95% (Teste t-Student). Desta forma, o método desenvolvido empregando LC-ICP-MS e LC-CVG-ICP-MS foi considerado adequado para determinação de espécies de As em moluscos bivalves.Coordenação de Aperfeiçoamento de Pessoal de Nível Superiorapplication/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em QuímicaUFSMBRQuímicaEspeciaçãoSpeciation scienceAmostras biológicasCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAEspécies de arsênio em moluscos bivalves determinadas por LC-ICP-MS E LC-CVG-ICP-MS após extração assistida por microondasinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisDressler, Valderi Luizhttp://lattes.cnpq.br/4054740296547580Borges, Daniel Lázaro Gallindohttp://lattes.cnpq.br/9529870514669368Moraes, Diogo Pompéu dehttp://lattes.cnpq.br/3777062632260326Silva, Fabiana Ernestina Barcellos dahttp://lattes.cnpq.br/3992443023418750Mesko, Márcia Fosterhttp://lattes.cnpq.br/2461255030745891http://lattes.cnpq.br/5084194130501067Santos, Clarissa Marques Moreira dos10060000000040030030030030030030029c59cfe-a489-425c-88a5-18fdf7cbf2585fe92bdc-d607-4a67-8a82-36abc5ff2101e05e117f-9066-40a8-96e6-7780e2db74f8f14a305a-1edb-4607-8511-83ac44280348b2f50313-d9c3-4715-a5b5-cdaeb9a99f20f4f59694-8614-4813-b490-f750c0e68be1info:eu-repo/semantics/openAccessreponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALMOREIRA, CLARISSA MARQUES.pdfapplication/pdf3387098http://repositorio.ufsm.br/bitstream/1/4249/1/MOREIRA%2c%20CLARISSA%20MARQUES.pdfd690d8a1aba445cd921f3f87cf72a91bMD51TEXTMOREIRA, CLARISSA MARQUES.pdf.txtMOREIRA, CLARISSA MARQUES.pdf.txtExtracted texttext/plain257893http://repositorio.ufsm.br/bitstream/1/4249/2/MOREIRA%2c%20CLARISSA%20MARQUES.pdf.txtdb0dbf3a1d5d6c5d0e46bb04ad612115MD52THUMBNAILMOREIRA, CLARISSA MARQUES.pdf.jpgMOREIRA, CLARISSA MARQUES.pdf.jpgIM Thumbnailimage/jpeg5962http://repositorio.ufsm.br/bitstream/1/4249/3/MOREIRA%2c%20CLARISSA%20MARQUES.pdf.jpg73e75987f99839495c3c6b6db5879c88MD531/42492023-06-12 14:12:26.866oai:repositorio.ufsm.br:1/4249Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2023-06-12T17:12:26Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Espécies de arsênio em moluscos bivalves determinadas por LC-ICP-MS E LC-CVG-ICP-MS após extração assistida por microondas |
title |
Espécies de arsênio em moluscos bivalves determinadas por LC-ICP-MS E LC-CVG-ICP-MS após extração assistida por microondas |
spellingShingle |
Espécies de arsênio em moluscos bivalves determinadas por LC-ICP-MS E LC-CVG-ICP-MS após extração assistida por microondas Santos, Clarissa Marques Moreira dos Especiação Speciation science Amostras biológicas CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Espécies de arsênio em moluscos bivalves determinadas por LC-ICP-MS E LC-CVG-ICP-MS após extração assistida por microondas |
title_full |
Espécies de arsênio em moluscos bivalves determinadas por LC-ICP-MS E LC-CVG-ICP-MS após extração assistida por microondas |
title_fullStr |
Espécies de arsênio em moluscos bivalves determinadas por LC-ICP-MS E LC-CVG-ICP-MS após extração assistida por microondas |
title_full_unstemmed |
Espécies de arsênio em moluscos bivalves determinadas por LC-ICP-MS E LC-CVG-ICP-MS após extração assistida por microondas |
title_sort |
Espécies de arsênio em moluscos bivalves determinadas por LC-ICP-MS E LC-CVG-ICP-MS após extração assistida por microondas |
author |
Santos, Clarissa Marques Moreira dos |
author_facet |
Santos, Clarissa Marques Moreira dos |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Dressler, Valderi Luiz |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/4054740296547580 |
dc.contributor.referee1.fl_str_mv |
Borges, Daniel Lázaro Gallindo |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/9529870514669368 |
dc.contributor.referee2.fl_str_mv |
Moraes, Diogo Pompéu de |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/3777062632260326 |
dc.contributor.referee3.fl_str_mv |
Silva, Fabiana Ernestina Barcellos da |
dc.contributor.referee3Lattes.fl_str_mv |
http://lattes.cnpq.br/3992443023418750 |
dc.contributor.referee4.fl_str_mv |
Mesko, Márcia Foster |
dc.contributor.referee4Lattes.fl_str_mv |
http://lattes.cnpq.br/2461255030745891 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/5084194130501067 |
dc.contributor.author.fl_str_mv |
Santos, Clarissa Marques Moreira dos |
contributor_str_mv |
Dressler, Valderi Luiz Borges, Daniel Lázaro Gallindo Moraes, Diogo Pompéu de Silva, Fabiana Ernestina Barcellos da Mesko, Márcia Foster |
dc.subject.por.fl_str_mv |
Especiação Speciation science Amostras biológicas |
topic |
Especiação Speciation science Amostras biológicas CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this work, the aim of this study is to evaluate sample preparation procedures and liquid chromatography-inductively coupled plasma mass spectrometry (LC-ICP-MS) and LC coupled to chemical vapor generation (CVG) and ICP-MS (LC-CVG-ICP-MS) for identification and quantification of As species in mollusks collected in BTS. Conditions related to As species extraction were assessed with the use of microwave assisted extraction (MAE) and ultrasound-assisted extraction (UAE). The influence of the main parameters involved in extraction of As species such as the type and concentration of extraction solution, sample mass, temperature and extraction time were evaluated. The extraction was possible by using water at 80 °C (0.2 g sample and 6 mL of w ater) for 6 min using MAE. For the chromatographic separation the type of mobile phase [(NH4)2CO3 and (NH4)2HPO4] concentration (1 to 20 mmol L-1), pH (5.0 to 9.0), flow rate (1.05 to 1.45 mL min-1) and elution mode (isocratic and gradient) were evaluated. The volume of sample injected into the chromatograph was fixed to 200 μL. For the separation of As species an anion exchange column (Hamilton PRP-X100, 250 x 4.1 mm) was used. Six As species were detected in the mollusks being identified arsenobetaine (AsB), As(III), dimethylarsenic acid (DMA) and ρ- arsanilic acid (ρ-ASA). The best separation of the As species was obtained by gradient elution mode and using the following program: 0 to 1.4 min using 6 mmol L-1 (NH4)2HPO4 to 1.4 to 2.7 min using 20 mmol L-1 (NH4)2CO3 and 2.7 to 15 min using 6 mmol L-1 (NH4)2HPO4). The mobile phase flow rate was set at 1.25 mL min-1. CVG parameters were evaluated and the concentrations of NaBH4 and HCl, and carrier gas flow rate were set to 1.0% (m/v) 1.0 mol L-1 and 1.15 L min-1, respectively. The extraction procedures and determination of total As were evaluated using certified reference materials BCR 627 (Tuna Fish Tissue), DORM-2 (Dogfish Muscle) and NIST 1566b (Oyster tissue). The agreement of the results obtained was 95 ± 3 to 101 ± 5%, respectively. The sum of the concentrations of As species determined by LC-ICP-MS and the total As concentration in digested samples and extracts measured, determined by ICP OES were also in good agreement on a confidence level of 95% (Student t-Test). The developed methods by employing the LC-ICP-MS and LC-CVGICP- MS for As speciation analyses in bivalves mollusks are considered suitable. |
publishDate |
2013 |
dc.date.issued.fl_str_mv |
2013-03-05 |
dc.date.accessioned.fl_str_mv |
2017-05-11 |
dc.date.available.fl_str_mv |
2017-05-11 |
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info:eu-repo/semantics/publishedVersion |
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info:eu-repo/semantics/doctoralThesis |
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doctoralThesis |
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publishedVersion |
dc.identifier.citation.fl_str_mv |
SANTOS, Clarissa Marques Moreira dos. Espécies de arsênio em moluscos bivalves determinadas por LC-ICP-MS E LC-CVG-ICP-MS após extração assistida por microondas. 2013. 155 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013. |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/4249 |
identifier_str_mv |
SANTOS, Clarissa Marques Moreira dos. Espécies de arsênio em moluscos bivalves determinadas por LC-ICP-MS E LC-CVG-ICP-MS após extração assistida por microondas. 2013. 155 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013. |
url |
http://repositorio.ufsm.br/handle/1/4249 |
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por |
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100600000000 |
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Universidade Federal de Santa Maria |
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UFSM |
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Química |
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Universidade Federal de Santa Maria |
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