Desenvolvimento de métodos utilizando HS-SPME/CG-EM para análise de HPAs em cafés

Detalhes bibliográficos
Ano de defesa: 2022
Autor(a) principal: Martins, Fátima Itana Chaves Custódio
Orientador(a): Nascimento, Ronaldo Ferreira do
Banca de defesa: Não Informado pela instituição
Tipo de documento: Tese
Tipo de acesso: Acesso aberto
Idioma: por
Instituição de defesa: Não Informado pela instituição
Programa de Pós-Graduação: Não Informado pela instituição
Departamento: Não Informado pela instituição
País: Não Informado pela instituição
Palavras-chave em Português:
Link de acesso: http://www.repositorio.ufc.br/handle/riufc/69950
Resumo: Coffee is one of the most commercialized beverages in the world. According data from the International Coffee Organization, Brazil is the world's largest producer and exporter. Although some studies have pointed out the benefits of coffee for human health, the toxic properties of coffees are still not completely understood. It is understood that during the process of roasting your grains, the formation of several potentially carcinogenic substances can occur, including polycyclic aromatic hydrocarbons (PAHs), which are associated with the incidence of cancer in humans due to their mutagenic and carcinogenic potential. In addition, it is important to note that the chemical composition of coffee may change due to variations in the quality of the beans, thereby influencing its cytotoxic, mutagenic and genotoxic potential. This study aimed to perform qualitative and quantitative analysis of PAHs in coffee samples, using solid phase microextraction (SPME) and Gas Chromatography coupled to Mass Spectrometry (GC-MS) as well as to evaluate the presence profile and the levels of 16 priority PAHs in powdered coffees and drink preparations of high quality and common quality of these compounds in coffee preparations via chemometric method of multivariate analysis by principal component analysis (PCA). Ten samples of powdered coffee were used, divided into commercial and special quality samples. Samples were enumerated with codes so as not to reveal the manufacturers. High quality samples: AC, CL, O, H and ME and common quality samples: TC, SC, ML, PIL and KM, all from Brazilian producers. All samples belong to the species Coffea arabica. The preparation of the drinks was done with distilled water and following the instructions on the labels. The method was validated according to the parameters selectivity, linearity, detection limit (LD), quantification limit (LQ), precision and accuracy, the latter in terms of recovered percentage. Student's t test and Hartley's F test were applied to verify the significance of the parameters and the regression of the analytical curves obtained in the coffee matrix. The method for determining PAHs proved to be well suited for all sample determinations (analysis of powdered coffee, analysis of beverages prepared by infusion and cooking) and, in addition to being fast and sensitive, it uses a low amount of toxic solvents. The intra-run accuracies were in the range of 11-21%, 8-18% and 6-17%, respectively, for the levels 1, 2 and 3 evaluated. The detection limit and the quantification limit established for the analytes were lower than 0.39-2.02 μg kg-1 and 1.20-6.48 μg kg-1, respectively. PAH recoveries ranged from 53 to 126%, with a relative standard deviation < 20%. The method proved to be efficient when applied to detect and quantify 16 PAHs in 3 coffee samples obtained by different preparations. In high-quality samples were observed average concentrations of 0.9 to 1.4 μg kg-1 and 0.6 to 0.7 μg kg-1, respectively for naphthalene and fluorene and up to 2.8 μg kg-1 for fluoranthene. In samples of common quality in addition to the PAHs already mentioned, the compounds dibenzo[a,h]anthracene (averages 0.9 and 1.3 μg kg-1), benzo[g,h,i]perylene (0.5 to 1.4 μg kg-1) and indene were quantified in two samples indene[1,2,3-cd]pyrene (average of 1.3 μg kg-1 in samples obtained by infusion). The analyzes showed that high quality coffees in general showed a predominance of compounds with lower numbers of aromatic rings, while samples of common quality showed levels of compounds with a higher number of rings, with appreciable concentrations of PAHs with pentose ring, the which characterizes the addition of “non-coffee products” during manufacture.
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spelling Martins, Fátima Itana Chaves CustódioNascimento, Ronaldo Ferreira do2023-01-02T18:28:59Z2023-01-02T18:28:59Z2022MARTINS, Fátima Itana Chaves Custódio. Desenvolvimento de método utilizando HS-SPME/GC-MS para análise de HPAs em cafés. 2022. 139 f. Tese (Doutorado em Química) - Universidade Federal do Ceará, Fortaleza, 2022.http://www.repositorio.ufc.br/handle/riufc/69950Coffee is one of the most commercialized beverages in the world. According data from the International Coffee Organization, Brazil is the world's largest producer and exporter. Although some studies have pointed out the benefits of coffee for human health, the toxic properties of coffees are still not completely understood. It is understood that during the process of roasting your grains, the formation of several potentially carcinogenic substances can occur, including polycyclic aromatic hydrocarbons (PAHs), which are associated with the incidence of cancer in humans due to their mutagenic and carcinogenic potential. In addition, it is important to note that the chemical composition of coffee may change due to variations in the quality of the beans, thereby influencing its cytotoxic, mutagenic and genotoxic potential. This study aimed to perform qualitative and quantitative analysis of PAHs in coffee samples, using solid phase microextraction (SPME) and Gas Chromatography coupled to Mass Spectrometry (GC-MS) as well as to evaluate the presence profile and the levels of 16 priority PAHs in powdered coffees and drink preparations of high quality and common quality of these compounds in coffee preparations via chemometric method of multivariate analysis by principal component analysis (PCA). Ten samples of powdered coffee were used, divided into commercial and special quality samples. Samples were enumerated with codes so as not to reveal the manufacturers. High quality samples: AC, CL, O, H and ME and common quality samples: TC, SC, ML, PIL and KM, all from Brazilian producers. All samples belong to the species Coffea arabica. The preparation of the drinks was done with distilled water and following the instructions on the labels. The method was validated according to the parameters selectivity, linearity, detection limit (LD), quantification limit (LQ), precision and accuracy, the latter in terms of recovered percentage. Student's t test and Hartley's F test were applied to verify the significance of the parameters and the regression of the analytical curves obtained in the coffee matrix. The method for determining PAHs proved to be well suited for all sample determinations (analysis of powdered coffee, analysis of beverages prepared by infusion and cooking) and, in addition to being fast and sensitive, it uses a low amount of toxic solvents. The intra-run accuracies were in the range of 11-21%, 8-18% and 6-17%, respectively, for the levels 1, 2 and 3 evaluated. The detection limit and the quantification limit established for the analytes were lower than 0.39-2.02 μg kg-1 and 1.20-6.48 μg kg-1, respectively. PAH recoveries ranged from 53 to 126%, with a relative standard deviation < 20%. The method proved to be efficient when applied to detect and quantify 16 PAHs in 3 coffee samples obtained by different preparations. In high-quality samples were observed average concentrations of 0.9 to 1.4 μg kg-1 and 0.6 to 0.7 μg kg-1, respectively for naphthalene and fluorene and up to 2.8 μg kg-1 for fluoranthene. In samples of common quality in addition to the PAHs already mentioned, the compounds dibenzo[a,h]anthracene (averages 0.9 and 1.3 μg kg-1), benzo[g,h,i]perylene (0.5 to 1.4 μg kg-1) and indene were quantified in two samples indene[1,2,3-cd]pyrene (average of 1.3 μg kg-1 in samples obtained by infusion). The analyzes showed that high quality coffees in general showed a predominance of compounds with lower numbers of aromatic rings, while samples of common quality showed levels of compounds with a higher number of rings, with appreciable concentrations of PAHs with pentose ring, the which characterizes the addition of “non-coffee products” during manufacture.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES), 48 meses de bolsaO café é uma das bebidas mais comercializadas mundialmente. Segundo dados da Organização Internacional do Café, o Brasil é o maior produtor e exportador mundial. Embora alguns estudos apontem os benefícios do café para a saúde humana, as propriedades tóxicas dessa bebida ainda não estão completamente esclarecidas. Entende-se que durante o processo de torrefação dos seus grãos pode ocorrer a formação de diversas substâncias potencialmente carcinogênicas, dentre elas os hidrocarbonetos policíclicos aromáticos (HPAs), os quais estão associados à incidência de câncer em seres humanos devido ao seu potencial mutagênico e carcinogênico. Além disso, é importante salientar que a composição química do café pode sofrer mudanças em decorrência das variações da qualidade dos grãos, influenciando dessa forma seu potencial citotóxico, mutagênico e genotóxico. Esse estudo objetivou realizar análises qualitativa e quantitativa de HPAs em amostras de café, usando microextração em fase sólida (SPME) e Cromatografia Gasosa acoplada a Espectrometria de Massas (CG-EM). Neste caso, foi avaliado o perfil de 16 HPAs em amostras de cafés em pó e preparação da bebida (de marcas de alta qualidade e qualidade comum), via análise multivariada por componentes principais (PCA). Foram utilizadas 10 amostras de café em pó (de alta qualidade e comum). As amostras foram codificadas para proteção das empresas. Amostras de alta qualidade: AC, CL, O, H e ME e amostras de qualidade comum: TC, SC, ML, PIL e KM, todas de produtores brasileiros. Todas as amostras pertencem à espécie Coffea arabica. As bebidas foram preparadas com água destilada e seguindo as instruções dos rótulos dos produtos. O método adaptado foi validado de acordo com os parâmetros seletividade, linearidade, limite de detecção (LD), limite de quantificação (LQ), precisão e exatidão (recuperação). Os testes estatísticos, de Student e F de Hartley, foram aplicados para verificar as significâncias dos coeficientes (linear, angular e determinação) das curvas analíticas obtidas na matriz de café. O método analítico usado para a determinação dos HPA’s revelou ser bem adequado para todas as amostras (café em pó, bebidas preparadas por infusão e por cozimento), além de ser rápido, sensível e baixo consumo de solventes tóxicos. A precisão (intra-corrida) foi satisfatória, na faixa de 11-21%, 8-18% e 6-17%, respectivamente, para três níveis avaliados. Os limites de detecção e o de quantificação estabelecidos para os analitos foram na faixa de 0.39-2.02 μg.kg-1 e 1.20-6.48 μg kg-1, respectivamente. As recuperações dos HPAs variaram de 53% a 126%, com um coeficiente de variação < 20%. O método se mostrou eficiente quando aplicado para detectar e quantificar 16 HPAs nas 3 amostras de café. Nas amostras de alta qualidade observamos concentrações médias de 0,9 a 1,4 μg kg-1 e 0,6 a 0,7 μg kg-1, respectivamente para naftaleno e fluoreno e até 2,8 μg kg-1 para fluoranteno. Nas amostras de qualidade comum além dos HPAs já citados, foram quantificados em duas amostras os compostos dibenzo[ah]antraceno (médias de 0,9 e 1,3 μg kg-1), benzo[ghi]perileno (0,5 a 1,4 μg kg-1) e indeno[1,2,3-cd]pireno (média de 1,3 μg kg-1 em amostras obtidas por infusão). As análises mostraram que os cafés de alta qualidade apresentaram, em geral, predominância de compostos com menores números de anéis aromáticos, enquanto as amostras de qualidade comum apresentaram níveis de compostos com maior número de anéis, havendo concentrações apreciáveis de HPAs com anel de pentose, o que caracteriza a adição de “produtos não café” durante a fabricação.Hidrocarbonetos policíclicos aromáticosCaféCromatografia gasosaEspectrometria de massasDesenvolvimento de métodos utilizando HS-SPME/CG-EM para análise de HPAs em cafésMethod development using HS-SPME/GC-MS for analysis of PAHs in coffeesinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisporreponame:Repositório Institucional da Universidade Federal do Ceará (UFC)instname:Universidade Federal do Ceará (UFC)instacron:UFCinfo:eu-repo/semantics/openAccessLICENSElicense.txtlicense.txttext/plain; charset=utf-81748http://repositorio.ufc.br/bitstream/riufc/69950/4/license.txt8a4605be74aa9ea9d79846c1fba20a33MD54ORIGINAL2022_tese_ficcmartins_29-12.pdf2022_tese_ficcmartins_29-12.pdfapplication/pdf3180954http://repositorio.ufc.br/bitstream/riufc/69950/3/2022_tese_ficcmartins_29-12.pdf7cc7463bccd6e21c79b3ba97149439d0MD53riufc/699502024-06-06 09:07:44.36oai:repositorio.ufc.br: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Repositório InstitucionalPUBhttp://www.repositorio.ufc.br/ri-oai/requestbu@ufc.br || repositorio@ufc.bropendoar:2024-06-06T12:07:44Repositório Institucional da Universidade Federal do Ceará (UFC) - Universidade Federal do Ceará (UFC)false
dc.title.pt_BR.fl_str_mv Desenvolvimento de métodos utilizando HS-SPME/CG-EM para análise de HPAs em cafés
dc.title.en.pt_BR.fl_str_mv Method development using HS-SPME/GC-MS for analysis of PAHs in coffees
title Desenvolvimento de métodos utilizando HS-SPME/CG-EM para análise de HPAs em cafés
spellingShingle Desenvolvimento de métodos utilizando HS-SPME/CG-EM para análise de HPAs em cafés
Martins, Fátima Itana Chaves Custódio
Hidrocarbonetos policíclicos aromáticos
Café
Cromatografia gasosa
Espectrometria de massas
title_short Desenvolvimento de métodos utilizando HS-SPME/CG-EM para análise de HPAs em cafés
title_full Desenvolvimento de métodos utilizando HS-SPME/CG-EM para análise de HPAs em cafés
title_fullStr Desenvolvimento de métodos utilizando HS-SPME/CG-EM para análise de HPAs em cafés
title_full_unstemmed Desenvolvimento de métodos utilizando HS-SPME/CG-EM para análise de HPAs em cafés
title_sort Desenvolvimento de métodos utilizando HS-SPME/CG-EM para análise de HPAs em cafés
author Martins, Fátima Itana Chaves Custódio
author_facet Martins, Fátima Itana Chaves Custódio
author_role author
dc.contributor.author.fl_str_mv Martins, Fátima Itana Chaves Custódio
dc.contributor.advisor1.fl_str_mv Nascimento, Ronaldo Ferreira do
contributor_str_mv Nascimento, Ronaldo Ferreira do
dc.subject.por.fl_str_mv Hidrocarbonetos policíclicos aromáticos
Café
Cromatografia gasosa
Espectrometria de massas
topic Hidrocarbonetos policíclicos aromáticos
Café
Cromatografia gasosa
Espectrometria de massas
description Coffee is one of the most commercialized beverages in the world. According data from the International Coffee Organization, Brazil is the world's largest producer and exporter. Although some studies have pointed out the benefits of coffee for human health, the toxic properties of coffees are still not completely understood. It is understood that during the process of roasting your grains, the formation of several potentially carcinogenic substances can occur, including polycyclic aromatic hydrocarbons (PAHs), which are associated with the incidence of cancer in humans due to their mutagenic and carcinogenic potential. In addition, it is important to note that the chemical composition of coffee may change due to variations in the quality of the beans, thereby influencing its cytotoxic, mutagenic and genotoxic potential. This study aimed to perform qualitative and quantitative analysis of PAHs in coffee samples, using solid phase microextraction (SPME) and Gas Chromatography coupled to Mass Spectrometry (GC-MS) as well as to evaluate the presence profile and the levels of 16 priority PAHs in powdered coffees and drink preparations of high quality and common quality of these compounds in coffee preparations via chemometric method of multivariate analysis by principal component analysis (PCA). Ten samples of powdered coffee were used, divided into commercial and special quality samples. Samples were enumerated with codes so as not to reveal the manufacturers. High quality samples: AC, CL, O, H and ME and common quality samples: TC, SC, ML, PIL and KM, all from Brazilian producers. All samples belong to the species Coffea arabica. The preparation of the drinks was done with distilled water and following the instructions on the labels. The method was validated according to the parameters selectivity, linearity, detection limit (LD), quantification limit (LQ), precision and accuracy, the latter in terms of recovered percentage. Student's t test and Hartley's F test were applied to verify the significance of the parameters and the regression of the analytical curves obtained in the coffee matrix. The method for determining PAHs proved to be well suited for all sample determinations (analysis of powdered coffee, analysis of beverages prepared by infusion and cooking) and, in addition to being fast and sensitive, it uses a low amount of toxic solvents. The intra-run accuracies were in the range of 11-21%, 8-18% and 6-17%, respectively, for the levels 1, 2 and 3 evaluated. The detection limit and the quantification limit established for the analytes were lower than 0.39-2.02 μg kg-1 and 1.20-6.48 μg kg-1, respectively. PAH recoveries ranged from 53 to 126%, with a relative standard deviation < 20%. The method proved to be efficient when applied to detect and quantify 16 PAHs in 3 coffee samples obtained by different preparations. In high-quality samples were observed average concentrations of 0.9 to 1.4 μg kg-1 and 0.6 to 0.7 μg kg-1, respectively for naphthalene and fluorene and up to 2.8 μg kg-1 for fluoranthene. In samples of common quality in addition to the PAHs already mentioned, the compounds dibenzo[a,h]anthracene (averages 0.9 and 1.3 μg kg-1), benzo[g,h,i]perylene (0.5 to 1.4 μg kg-1) and indene were quantified in two samples indene[1,2,3-cd]pyrene (average of 1.3 μg kg-1 in samples obtained by infusion). The analyzes showed that high quality coffees in general showed a predominance of compounds with lower numbers of aromatic rings, while samples of common quality showed levels of compounds with a higher number of rings, with appreciable concentrations of PAHs with pentose ring, the which characterizes the addition of “non-coffee products” during manufacture.
publishDate 2022
dc.date.issued.fl_str_mv 2022
dc.date.accessioned.fl_str_mv 2023-01-02T18:28:59Z
dc.date.available.fl_str_mv 2023-01-02T18:28:59Z
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dc.identifier.citation.fl_str_mv MARTINS, Fátima Itana Chaves Custódio. Desenvolvimento de método utilizando HS-SPME/GC-MS para análise de HPAs em cafés. 2022. 139 f. Tese (Doutorado em Química) - Universidade Federal do Ceará, Fortaleza, 2022.
dc.identifier.uri.fl_str_mv http://www.repositorio.ufc.br/handle/riufc/69950
identifier_str_mv MARTINS, Fátima Itana Chaves Custódio. Desenvolvimento de método utilizando HS-SPME/GC-MS para análise de HPAs em cafés. 2022. 139 f. Tese (Doutorado em Química) - Universidade Federal do Ceará, Fortaleza, 2022.
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