Determinação simultânea de ferro e níquel em suplementos alimentares por HR-CS SS-GF AAS
Ano de defesa: | 2019 |
---|---|
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 Santa Maria
Centro de Ciências Naturais e Exatas |
Programa de Pós-Graduação: |
Programa de Pós-Graduação em Química
|
Departamento: |
Química
|
País: |
Brasil
|
Palavras-chave em Português: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/17192 |
Resumo: | In this work a method was developed for the simultaneous determination of Fe and Ni as contaminants in dietary supplements by high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sample analysis (HR-CS SS-GF AAS). Measurements were done with the secondary lines of Ni and Fe at 352.454 nm and 352.604 nm, respectively, to avoid spectral interferences. The peak volume selected absorbance (PVSA), obtained from the sum of the integrated absorbance values of the center pixel plus the four adjacent ones (CP ± 2) was used as an analytical signal for the quantification of the elements. The best temperatures for pyrolysis and atomization for Fe and Ni were 1000 and 2700 °C, respectively. The use of chemical modifiers was not necessary and no matrix effects were observed. The samples were considered sufficiently homogeneous, since the calculated homogeneity factor was less than 10. Sample mass ranged from 0.25 to 2.8 mg depending on the type of the sample. To compare the measurements performed with different sample masses, the PVSA was normalized for a sample mass of 1 mg. Calibration curves for both analytes were obtained simultaneously, using aqueous standard solutions and standard addition method, for comparison for both calibration modes. The limit of detection was 514 ng g-1 for Fe and 11 ng g-1 for Ni. The precision ranged from 1.33 to 5.57% and from 4.31 to 9.21% for Fe and Ni, respectively. The method accuracy was assessed with recovery experiments and statistical comparison between the analytes concentrations, which were obtained by measurement solid samples with the proposed method and after digestion of the samples. The recoveries ranged from 91.2 to 106.3% for Fe and 75.9 to 111.7% for Ni when the samples were fortified with 5, 7.5 and 10 ng of Fe and 50, 75 and 100 pg of Ni and measured by the proposed method. The proposed methodology was successfully applied to determine both metals in different dietary supplements. |
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2019-06-28T12:18:17Z2019-06-28T12:18:17Z2019-02-26http://repositorio.ufsm.br/handle/1/17192In this work a method was developed for the simultaneous determination of Fe and Ni as contaminants in dietary supplements by high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sample analysis (HR-CS SS-GF AAS). Measurements were done with the secondary lines of Ni and Fe at 352.454 nm and 352.604 nm, respectively, to avoid spectral interferences. The peak volume selected absorbance (PVSA), obtained from the sum of the integrated absorbance values of the center pixel plus the four adjacent ones (CP ± 2) was used as an analytical signal for the quantification of the elements. The best temperatures for pyrolysis and atomization for Fe and Ni were 1000 and 2700 °C, respectively. The use of chemical modifiers was not necessary and no matrix effects were observed. The samples were considered sufficiently homogeneous, since the calculated homogeneity factor was less than 10. Sample mass ranged from 0.25 to 2.8 mg depending on the type of the sample. To compare the measurements performed with different sample masses, the PVSA was normalized for a sample mass of 1 mg. Calibration curves for both analytes were obtained simultaneously, using aqueous standard solutions and standard addition method, for comparison for both calibration modes. The limit of detection was 514 ng g-1 for Fe and 11 ng g-1 for Ni. The precision ranged from 1.33 to 5.57% and from 4.31 to 9.21% for Fe and Ni, respectively. The method accuracy was assessed with recovery experiments and statistical comparison between the analytes concentrations, which were obtained by measurement solid samples with the proposed method and after digestion of the samples. The recoveries ranged from 91.2 to 106.3% for Fe and 75.9 to 111.7% for Ni when the samples were fortified with 5, 7.5 and 10 ng of Fe and 50, 75 and 100 pg of Ni and measured by the proposed method. The proposed methodology was successfully applied to determine both metals in different dietary supplements.Neste trabalho foi desenvolvido um método para a determinação simultânea de Fe e Ni como contaminantes em suplementos alimentares por espectrometria de absorção atômica de alta resolução com fonte contínua em forno de grafite e amostragem direta de sólidos (HR-CS SS-GF AAS). As medidas foram feitas utilizando as linhas secundárias de Ni e Fe em 352.454 nm e 352.604 nm, respectivamente, para evitar interferências espectrais. A absorvância selecionada do volume de pico (PVSA), obtida a partir da soma dos valores de absorvância integrada do pixel central mais quatro pixels adjacentes (CP±2) foi usada como sinal analítico para quantificação dos elementos. As melhores temperaturas de pirólise e atomização para Fe e Ni foram 1000 e 2700 °C, respectivamente. O uso de modificadores químicos não foi necessário e nenhum efeito de matriz foi observado. As amostras foram consideradas suficientemente homogêneas, uma vez que o fator de homogeneidade calculado foi inferior a 10. O intervalo de massa utilizado variou de 0,25 a 2,8 mg dependendo do tipo de amostra. Para comparar as medidas realizadas com diferentes massas de amostra, a PVSA foi normalizada para uma massa de amostra de 1 mg. As curvas de calibração para ambos os analitos foram obtidas simultaneamente, utilizando soluções padrões aquosas e pela técnica de adição do analito, para comparação de ambos os modos de calibração. Os limites de detecção foram 514 ng g-1 para Fe e 11 ng g-1 para Ni. A precisão variou de 1,33 a 5,57% e de 4,31 a 9,21% para Fe e Ni, respectivamente. A exatidão do método foi avaliada com experimentos de recuperação e comparação estatística entre as concentrações dos analitos, que foram obtidas por meio da análise das amostras sólidas com o método proposto e após a digestão das amostras. As recuperações variaram de 91,2 a 106,3 % para Fe e 75,9 a 111,7 % para Ni quando as amostras foram fortificadas com 5, 7,5 e 10 ng de Fe e 50, 75 e 100 pg de Ni e medidas pelo método proposto. A metodologia proposta foi aplicada com sucesso para determinar ambos os metais em diferentes suplementos alimentares.porUniversidade Federal de Santa MariaCentro de Ciências Naturais e ExatasPrograma de Pós-Graduação em QuímicaUFSMBrasilQuímicaAttribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/info:eu-repo/semantics/openAccessDeterminação simultâneaAmostragem sólidaSuplementos alimentaresContaminaçãoFerroNíquelHR-CS SS-GF AASSimultaneous determinationSolid samplingDietary supplementsContaminationIronNickelCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação simultânea de ferro e níquel em suplementos alimentares por HR-CS SS-GF AASSimultaneous determination of iron and nickel in dietary supplements by HR-CS SS-GF AASinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisNascimento, Paulo Cícero dohttp://lattes.cnpq.br/7151513617218161Silva, Carine Vianahttp://lattes.cnpq.br/2004872342535591Dessuy, Morgana Bazzanhttp://lattes.cnpq.br/2433844803067772http://lattes.cnpq.br/9341103836347299Adolfo, Franciéle Rovasi100600000000600578b51ed-b12f-4664-9b87-387ad073b32c5819643b-01f8-4fc3-9bd9-bc684b572652c44ed480-6f9b-46d9-b4d3-efeb255f4951fe1fc97b-7cb3-42f5-8b48-2df599279015reponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUIMICA_2019_ADOLFO_FRANCIELE.pdfDIS_PPGQUIMICA_2019_ADOLFO_FRANCIELE.pdfDissertação de Mestradoapplication/pdf3748359http://repositorio.ufsm.br/bitstream/1/17192/1/DIS_PPGQUIMICA_2019_ADOLFO_FRANCIELE.pdf017f84b9365cebb1db5474ce067139d9MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Determinação simultânea de ferro e níquel em suplementos alimentares por HR-CS SS-GF AAS |
dc.title.alternative.eng.fl_str_mv |
Simultaneous determination of iron and nickel in dietary supplements by HR-CS SS-GF AAS |
title |
Determinação simultânea de ferro e níquel em suplementos alimentares por HR-CS SS-GF AAS |
spellingShingle |
Determinação simultânea de ferro e níquel em suplementos alimentares por HR-CS SS-GF AAS Adolfo, Franciéle Rovasi Determinação simultânea Amostragem sólida Suplementos alimentares Contaminação Ferro Níquel HR-CS SS-GF AAS Simultaneous determination Solid sampling Dietary supplements Contamination Iron Nickel CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação simultânea de ferro e níquel em suplementos alimentares por HR-CS SS-GF AAS |
title_full |
Determinação simultânea de ferro e níquel em suplementos alimentares por HR-CS SS-GF AAS |
title_fullStr |
Determinação simultânea de ferro e níquel em suplementos alimentares por HR-CS SS-GF AAS |
title_full_unstemmed |
Determinação simultânea de ferro e níquel em suplementos alimentares por HR-CS SS-GF AAS |
title_sort |
Determinação simultânea de ferro e níquel em suplementos alimentares por HR-CS SS-GF AAS |
author |
Adolfo, Franciéle Rovasi |
author_facet |
Adolfo, Franciéle Rovasi |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Nascimento, Paulo Cícero do |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/7151513617218161 |
dc.contributor.referee1.fl_str_mv |
Silva, Carine Viana |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/2004872342535591 |
dc.contributor.referee2.fl_str_mv |
Dessuy, Morgana Bazzan |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/2433844803067772 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/9341103836347299 |
dc.contributor.author.fl_str_mv |
Adolfo, Franciéle Rovasi |
contributor_str_mv |
Nascimento, Paulo Cícero do Silva, Carine Viana Dessuy, Morgana Bazzan |
dc.subject.por.fl_str_mv |
Determinação simultânea Amostragem sólida Suplementos alimentares Contaminação Ferro Níquel HR-CS SS-GF AAS |
topic |
Determinação simultânea Amostragem sólida Suplementos alimentares Contaminação Ferro Níquel HR-CS SS-GF AAS Simultaneous determination Solid sampling Dietary supplements Contamination Iron Nickel CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Simultaneous determination Solid sampling Dietary supplements Contamination Iron Nickel |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this work a method was developed for the simultaneous determination of Fe and Ni as contaminants in dietary supplements by high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sample analysis (HR-CS SS-GF AAS). Measurements were done with the secondary lines of Ni and Fe at 352.454 nm and 352.604 nm, respectively, to avoid spectral interferences. The peak volume selected absorbance (PVSA), obtained from the sum of the integrated absorbance values of the center pixel plus the four adjacent ones (CP ± 2) was used as an analytical signal for the quantification of the elements. The best temperatures for pyrolysis and atomization for Fe and Ni were 1000 and 2700 °C, respectively. The use of chemical modifiers was not necessary and no matrix effects were observed. The samples were considered sufficiently homogeneous, since the calculated homogeneity factor was less than 10. Sample mass ranged from 0.25 to 2.8 mg depending on the type of the sample. To compare the measurements performed with different sample masses, the PVSA was normalized for a sample mass of 1 mg. Calibration curves for both analytes were obtained simultaneously, using aqueous standard solutions and standard addition method, for comparison for both calibration modes. The limit of detection was 514 ng g-1 for Fe and 11 ng g-1 for Ni. The precision ranged from 1.33 to 5.57% and from 4.31 to 9.21% for Fe and Ni, respectively. The method accuracy was assessed with recovery experiments and statistical comparison between the analytes concentrations, which were obtained by measurement solid samples with the proposed method and after digestion of the samples. The recoveries ranged from 91.2 to 106.3% for Fe and 75.9 to 111.7% for Ni when the samples were fortified with 5, 7.5 and 10 ng of Fe and 50, 75 and 100 pg of Ni and measured by the proposed method. The proposed methodology was successfully applied to determine both metals in different dietary supplements. |
publishDate |
2019 |
dc.date.accessioned.fl_str_mv |
2019-06-28T12:18:17Z |
dc.date.available.fl_str_mv |
2019-06-28T12:18:17Z |
dc.date.issued.fl_str_mv |
2019-02-26 |
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/1/17192 |
url |
http://repositorio.ufsm.br/handle/1/17192 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 |
dc.relation.authority.fl_str_mv |
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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.publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
dc.publisher.program.fl_str_mv |
Programa de Pós-Graduação em Química |
dc.publisher.initials.fl_str_mv |
UFSM |
dc.publisher.country.fl_str_mv |
Brasil |
dc.publisher.department.fl_str_mv |
Química |
publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
dc.source.none.fl_str_mv |
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UFSM |
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