Método de preparo de amostras em câmara única de reação assistida por radiação micro-ondas e determinação de elementos terras raras em azeite de oliva extra virgem por USN-ICP-MS
Autor(a) principal: | |
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Data de Publicação: | 2022 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Repositório Institucional Manancial UFSM |
Texto Completo: | http://repositorio.ufsm.br/handle/1/29475 |
Resumo: | The rare earth elements (REE) present in extra virgin olive oil (EVOO) have been considered as studied markers for traceability of the production origin. However, REE are present in low concentrations (ng g-1 range) in EVOO, requiring analytical methods sufficient for multi-element determination and with low limits of quantification (LOQ). In addition, the conditions used in the method must minimize matrix and residual acidity (RA) interferences and digest a high mass of EVOO. Thus, the objective of this work was to propose a method for sample preparation of EVOO using microwave-assisted wet digestion in a single reaction chamber (MAWD-SRC) and determination of REE by inductively coupled plasma mass spectrometry with an ultrasonic nebulizer (USN-ICPMS). Initially, the irradiation program was evaluated to allow the digestion of high masses of EVOO (1.0 to 2.0 g). The optimized irradiation program conditions were: (i) 5 min ramp to 115 ºC; (ii) 50 min ramp to 180 ºC; (iii) 10 min ramp to 270 ºC, and hold for 20 min at 270 ºC. The initial pressure with Ar gas and power applied was 40 bar and 1500 W, respectively. The digestion efficiency was evaluated from dissolved organic carbon (DOC) and residual acidity (RA). Considering the complexity of the sample, such as the presence of organic compounds that are difficult to decompose, especially linoleic acid, it is necessary to use concentrated HNO3 employing the MAWD-SRC. Thus, the digestion of 1.0, 1.5 and 2.0 g of EVOO in 6, 7 and 8 mL of 14.4 mol L-1 HNO3 was evaluated. Using the optimized irradiation program was possible to digest up to 2.0 g of EVOO completely. The optimal condition for REE determination was obtained using 1.0 g of EVOO and 8 mL of 14.4 mol L-1 HNO3, resulting in DOC and RA of 129 mg L-1 and 7%, respectively, requiring a low dilution factor of the digests (4 times) to match the acidity content with the calibration solution. The accuracy was evaluated by adding REE to the samples from the reference solution before digestion, obtaining 90 to 107% recovery. Accuracy was also evaluated by comparing the results obtained with the proposed and the microwave-assisted wet digestion (MAWD) reference methods, and showed no statistical difference (t-test, with 95% confidence level) between the results. Moreover, MAWD-SRC allowed the efficient digestion of the high mass of EVOO (1 g) compared to MAWD (0.4 g). MAWDSRC enabled lower LOQ (0.01 - 0.7 ng g-1 ) than MAWD (0.1 - 6.8 ng g-1 ), favoring the quantification of more REE analytes at low concentrations. Therefore, the proposed method is efficient for REE determination at very low concentrations in EVOO and can be used in olive oil authenticity studies. |
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2023-06-16T13:45:34Z2023-06-16T13:45:34Z2022-12-16http://repositorio.ufsm.br/handle/1/29475The rare earth elements (REE) present in extra virgin olive oil (EVOO) have been considered as studied markers for traceability of the production origin. However, REE are present in low concentrations (ng g-1 range) in EVOO, requiring analytical methods sufficient for multi-element determination and with low limits of quantification (LOQ). In addition, the conditions used in the method must minimize matrix and residual acidity (RA) interferences and digest a high mass of EVOO. Thus, the objective of this work was to propose a method for sample preparation of EVOO using microwave-assisted wet digestion in a single reaction chamber (MAWD-SRC) and determination of REE by inductively coupled plasma mass spectrometry with an ultrasonic nebulizer (USN-ICPMS). Initially, the irradiation program was evaluated to allow the digestion of high masses of EVOO (1.0 to 2.0 g). The optimized irradiation program conditions were: (i) 5 min ramp to 115 ºC; (ii) 50 min ramp to 180 ºC; (iii) 10 min ramp to 270 ºC, and hold for 20 min at 270 ºC. The initial pressure with Ar gas and power applied was 40 bar and 1500 W, respectively. The digestion efficiency was evaluated from dissolved organic carbon (DOC) and residual acidity (RA). Considering the complexity of the sample, such as the presence of organic compounds that are difficult to decompose, especially linoleic acid, it is necessary to use concentrated HNO3 employing the MAWD-SRC. Thus, the digestion of 1.0, 1.5 and 2.0 g of EVOO in 6, 7 and 8 mL of 14.4 mol L-1 HNO3 was evaluated. Using the optimized irradiation program was possible to digest up to 2.0 g of EVOO completely. The optimal condition for REE determination was obtained using 1.0 g of EVOO and 8 mL of 14.4 mol L-1 HNO3, resulting in DOC and RA of 129 mg L-1 and 7%, respectively, requiring a low dilution factor of the digests (4 times) to match the acidity content with the calibration solution. The accuracy was evaluated by adding REE to the samples from the reference solution before digestion, obtaining 90 to 107% recovery. Accuracy was also evaluated by comparing the results obtained with the proposed and the microwave-assisted wet digestion (MAWD) reference methods, and showed no statistical difference (t-test, with 95% confidence level) between the results. Moreover, MAWD-SRC allowed the efficient digestion of the high mass of EVOO (1 g) compared to MAWD (0.4 g). MAWDSRC enabled lower LOQ (0.01 - 0.7 ng g-1 ) than MAWD (0.1 - 6.8 ng g-1 ), favoring the quantification of more REE analytes at low concentrations. Therefore, the proposed method is efficient for REE determination at very low concentrations in EVOO and can be used in olive oil authenticity studies.Os elementos terras raras (REE) presentes no azeite de oliva extra virgem (EVOO) têm sido considerados marcadores estudados para rastreabilidade da origem de produção do azeite. Entretanto, os REE estão presentes em baixas concentrações (faixa de ng g-1 ) no EVOO, exigindo métodos analíticos eficientes para determinação multielementar e com baixos limites de quantificação (LOQ). Além disso, é necessário que as condições utilizadas no método minimizem as interferências da matriz, da acidez residual (RA) e sejam capazes de decompor elevada massa do EVOO. Com isso, o objetivo deste trabalho foi propor um método de preparo de amostras de EVOO utilizando decomposição por via úmida assistida por radiação micro-ondas em câmara única de reação (MAWD-SRC) e determinação de REE por espectrometria de massa com plasma indutivamente acoplado com nebulizador ultrassônico (USN-ICP-MS). Inicialmente, o programa de irradiação foi avaliado para o favorecimento da decomposição de elevadas massas de EVOO (1,0 a 2,0 g). As condições otimizadas do programa de irradiação foram: (i) 5 minutos de rampa até 115 ºC; (ii) 50 minutos de rampa até 180 ºC; (iii) 10 minutos de rampa até 270 ºC, e permanência por 20 minutos em 270 ºC. A pressão inicial de Ar e potência aplicadas foram de 40 bar e 1500 W, respectivamente. A eficiência de decomposição dos digeridos foi avaliada a partir da determinação do carbono orgânico dissolvido (DOC) e acidez residual (RA). Considerando a complexidade da amostra, como a presença de compostos orgânicos de difícil decomposição, destacando-se o ácido linoleico, é necessário o uso de HNO3 concentrado empregando o método MAWD-SRC. Foram avaliadas a decomposição de 1, 1,5 e 2 g de EVOO com 6, 7 e 8 mL de HNO3 14,4 mol L-1 . Com o programa de irradiação otimizado, foi possível decompor completamente até 2 g de EVOO. A condição ótima para determinação de REE, foi obtida utilizando 1 g de EVOO e 8 mL de HNO3 14,4 mol L-1 , resultando em DOC e RA de 129 mg L-1 e 7%, respectivamente, requerendo um baixo fator de diluição dos digeridos (4 vezes) para adequar o teor de acidez com a solução de calibração. A exatidão foi avaliada pela adição de REE nas amostras a partir da solução de referência antes da decomposição, obtendo recuperação de 90% a 107%. A exatidão também foi avaliada comparando os resultados obtidos pelo método proposto e o método de referência, sendo a decomposição por via úmida assistida por radiação micro-ondas (MAWD). Não teve diferença estatística (teste-t, com nível de confiança de 95%) entre os resultados de REE após utilização de ambos os métodos. Além disso, a MAWD-SRC permitiu a decomposição eficiente de uma maior massa de EVOO (1 g) em comparação com a MAWD (0,4 g). A MAWD-SRC possibilitou menores LOQ (0,01 - 0,7 ng g-1 ) que a MAWD (0,1 - 6,8 ng g-1 ), favorecendo a quantificação de mais analitos REE em baixas concentrações. Portanto, o método proposto é eficiente para determinação de REE em concentrações muito baixas em EVOO, podendo ser utilizado em estudos de autenticidade de azeite de oliva.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/openAccessAzeite de olivaAutenticidadeElementos terras rarasPreparo de amostraICP-MSOlive oilAuthenticityRare earth elementsSample preparationCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAMétodo de preparo de amostras em câmara única de reação assistida por radiação micro-ondas e determinação de elementos terras raras em azeite de oliva extra virgem por USN-ICP-MSSample preparation method in single reaction chamber assisted by microwave radiation and determination of rare earth elements in extra virgin olive oil by USN-ICP-MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisSilva, Jussiane Souza dahttp://lattes.cnpq.br/8753473372692707Flores, Érico Marlon de MoraesFlores, Éder Lisandro de MoraesBizzi, Cezar Augustohttp://lattes.cnpq.br/3141054619235848Poletto, Bruno de Oliveira100600000000600600600600600600621bbbbe-cae3-4c4f-b58e-ab59fe37d9a121192d4e-3855-4791-8490-09f0de21763d554c6802-fa60-428b-831e-5bd78612061444b2e8e0-9f59-4bfc-9a22-9662db92dac8ea5d5aeb-956d-4091-b711-982595b3e995reponame:Repositório Institucional Manancial UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMCC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Método de preparo de amostras em câmara única de reação assistida por radiação micro-ondas e determinação de elementos terras raras em azeite de oliva extra virgem por USN-ICP-MS |
dc.title.alternative.eng.fl_str_mv |
Sample preparation method in single reaction chamber assisted by microwave radiation and determination of rare earth elements in extra virgin olive oil by USN-ICP-MS |
title |
Método de preparo de amostras em câmara única de reação assistida por radiação micro-ondas e determinação de elementos terras raras em azeite de oliva extra virgem por USN-ICP-MS |
spellingShingle |
Método de preparo de amostras em câmara única de reação assistida por radiação micro-ondas e determinação de elementos terras raras em azeite de oliva extra virgem por USN-ICP-MS Poletto, Bruno de Oliveira Azeite de oliva Autenticidade Elementos terras raras Preparo de amostra ICP-MS Olive oil Authenticity Rare earth elements Sample preparation CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Método de preparo de amostras em câmara única de reação assistida por radiação micro-ondas e determinação de elementos terras raras em azeite de oliva extra virgem por USN-ICP-MS |
title_full |
Método de preparo de amostras em câmara única de reação assistida por radiação micro-ondas e determinação de elementos terras raras em azeite de oliva extra virgem por USN-ICP-MS |
title_fullStr |
Método de preparo de amostras em câmara única de reação assistida por radiação micro-ondas e determinação de elementos terras raras em azeite de oliva extra virgem por USN-ICP-MS |
title_full_unstemmed |
Método de preparo de amostras em câmara única de reação assistida por radiação micro-ondas e determinação de elementos terras raras em azeite de oliva extra virgem por USN-ICP-MS |
title_sort |
Método de preparo de amostras em câmara única de reação assistida por radiação micro-ondas e determinação de elementos terras raras em azeite de oliva extra virgem por USN-ICP-MS |
author |
Poletto, Bruno de Oliveira |
author_facet |
Poletto, Bruno de Oliveira |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Silva, Jussiane Souza da |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/8753473372692707 |
dc.contributor.advisor-co1.fl_str_mv |
Flores, Érico Marlon de Moraes |
dc.contributor.referee1.fl_str_mv |
Flores, Éder Lisandro de Moraes |
dc.contributor.referee2.fl_str_mv |
Bizzi, Cezar Augusto |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/3141054619235848 |
dc.contributor.author.fl_str_mv |
Poletto, Bruno de Oliveira |
contributor_str_mv |
Silva, Jussiane Souza da Flores, Érico Marlon de Moraes Flores, Éder Lisandro de Moraes Bizzi, Cezar Augusto |
dc.subject.por.fl_str_mv |
Azeite de oliva Autenticidade Elementos terras raras Preparo de amostra ICP-MS |
topic |
Azeite de oliva Autenticidade Elementos terras raras Preparo de amostra ICP-MS Olive oil Authenticity Rare earth elements Sample preparation CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Olive oil Authenticity Rare earth elements Sample preparation |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
The rare earth elements (REE) present in extra virgin olive oil (EVOO) have been considered as studied markers for traceability of the production origin. However, REE are present in low concentrations (ng g-1 range) in EVOO, requiring analytical methods sufficient for multi-element determination and with low limits of quantification (LOQ). In addition, the conditions used in the method must minimize matrix and residual acidity (RA) interferences and digest a high mass of EVOO. Thus, the objective of this work was to propose a method for sample preparation of EVOO using microwave-assisted wet digestion in a single reaction chamber (MAWD-SRC) and determination of REE by inductively coupled plasma mass spectrometry with an ultrasonic nebulizer (USN-ICPMS). Initially, the irradiation program was evaluated to allow the digestion of high masses of EVOO (1.0 to 2.0 g). The optimized irradiation program conditions were: (i) 5 min ramp to 115 ºC; (ii) 50 min ramp to 180 ºC; (iii) 10 min ramp to 270 ºC, and hold for 20 min at 270 ºC. The initial pressure with Ar gas and power applied was 40 bar and 1500 W, respectively. The digestion efficiency was evaluated from dissolved organic carbon (DOC) and residual acidity (RA). Considering the complexity of the sample, such as the presence of organic compounds that are difficult to decompose, especially linoleic acid, it is necessary to use concentrated HNO3 employing the MAWD-SRC. Thus, the digestion of 1.0, 1.5 and 2.0 g of EVOO in 6, 7 and 8 mL of 14.4 mol L-1 HNO3 was evaluated. Using the optimized irradiation program was possible to digest up to 2.0 g of EVOO completely. The optimal condition for REE determination was obtained using 1.0 g of EVOO and 8 mL of 14.4 mol L-1 HNO3, resulting in DOC and RA of 129 mg L-1 and 7%, respectively, requiring a low dilution factor of the digests (4 times) to match the acidity content with the calibration solution. The accuracy was evaluated by adding REE to the samples from the reference solution before digestion, obtaining 90 to 107% recovery. Accuracy was also evaluated by comparing the results obtained with the proposed and the microwave-assisted wet digestion (MAWD) reference methods, and showed no statistical difference (t-test, with 95% confidence level) between the results. Moreover, MAWD-SRC allowed the efficient digestion of the high mass of EVOO (1 g) compared to MAWD (0.4 g). MAWDSRC enabled lower LOQ (0.01 - 0.7 ng g-1 ) than MAWD (0.1 - 6.8 ng g-1 ), favoring the quantification of more REE analytes at low concentrations. Therefore, the proposed method is efficient for REE determination at very low concentrations in EVOO and can be used in olive oil authenticity studies. |
publishDate |
2022 |
dc.date.issued.fl_str_mv |
2022-12-16 |
dc.date.accessioned.fl_str_mv |
2023-06-16T13:45:34Z |
dc.date.available.fl_str_mv |
2023-06-16T13:45:34Z |
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/1/29475 |
url |
http://repositorio.ufsm.br/handle/1/29475 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 600 600 600 600 600 |
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 |
reponame:Repositório Institucional Manancial UFSM instname:Universidade Federal de Santa Maria (UFSM) instacron:UFSM |
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Universidade Federal de Santa Maria (UFSM) |
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UFSM |
institution |
UFSM |
reponame_str |
Repositório Institucional Manancial UFSM |
collection |
Repositório Institucional Manancial UFSM |
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http://repositorio.ufsm.br/bitstream/1/29475/2/license_rdf http://repositorio.ufsm.br/bitstream/1/29475/3/license.txt http://repositorio.ufsm.br/bitstream/1/29475/1/DIS_PPGQU%c3%8dMICA_2022_POLETTO_BRUNO.pdf |
bitstream.checksum.fl_str_mv |
4460e5956bc1d1639be9ae6146a50347 2f0571ecee68693bd5cd3f17c1e075df 55a89afa0751faee098f30e081666ca3 |
bitstream.checksumAlgorithm.fl_str_mv |
MD5 MD5 MD5 |
repository.name.fl_str_mv |
Repositório Institucional Manancial UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
ouvidoria@ufsm.br |
_version_ |
1808854704249110528 |