Validação e determinação de patulina em suco de maçã utilizando cromatografia líquida acoplada a espectrometria de massa tandem
Autor(a) principal: | |
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Data de Publicação: | 2021 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Biblioteca Digital de Teses e Dissertações do UFSM |
Texto Completo: | http://repositorio.ufsm.br/handle/1/22734 |
Resumo: | Patulin (PAT) is a mycotoxin produced by certain fungal species which is frequently found contaminating apples and derived products, especially juice. Several fungal pathogens, in particular Penicillium species, have been identified as causative agents of diseases in apples. PAT contamination may occur due to reasons as geographic differences, climatic conditions, agricultural practices, cultivars and postharvest environment, which may affect fruit composition. This toxic contaminant is associated with mutagenic, immunosuppressive and neurotoxic effects in humans and animals. In Brazil and in the world effective control of PAT contamination depends on reliable analytical methods. This study developed and validated a technique for the analysis of PAT in samples of industrialized apple juice based on liquid-liquid extraction, using acetonitrile as the extraction solvent. Detection via mass spectrometry was performed after Atmospher Pressure Chemical Ionization (APCI). Mean recoveries of 97.5, 92.49 and 96.92% were reached for 4, 8 and 20 μg/L of PAT, respectively. The mean recovery of the method was 95.64%. The reproducibility of the presented methodology was confirmed when the results of a FAPAS proficiency test, showing a 95.9% recovery, in addition to presenting a good selectivity. The method uncertainty was estimated on three different days for three concentrations 4, 8 and 20 μg / L in replicates of 7 times each concentration, obtaining 0.37%, 6.62%The analyte was monitored with an APCI source in negative ion mode to identify its fragments. The 24 analyzed samples presented PAT levels below the limit of quantification. |
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2021-11-05T17:04:40Z2021-11-05T17:04:40Z2021-03-04http://repositorio.ufsm.br/handle/1/22734Patulin (PAT) is a mycotoxin produced by certain fungal species which is frequently found contaminating apples and derived products, especially juice. Several fungal pathogens, in particular Penicillium species, have been identified as causative agents of diseases in apples. PAT contamination may occur due to reasons as geographic differences, climatic conditions, agricultural practices, cultivars and postharvest environment, which may affect fruit composition. This toxic contaminant is associated with mutagenic, immunosuppressive and neurotoxic effects in humans and animals. In Brazil and in the world effective control of PAT contamination depends on reliable analytical methods. This study developed and validated a technique for the analysis of PAT in samples of industrialized apple juice based on liquid-liquid extraction, using acetonitrile as the extraction solvent. Detection via mass spectrometry was performed after Atmospher Pressure Chemical Ionization (APCI). Mean recoveries of 97.5, 92.49 and 96.92% were reached for 4, 8 and 20 μg/L of PAT, respectively. The mean recovery of the method was 95.64%. The reproducibility of the presented methodology was confirmed when the results of a FAPAS proficiency test, showing a 95.9% recovery, in addition to presenting a good selectivity. The method uncertainty was estimated on three different days for three concentrations 4, 8 and 20 μg / L in replicates of 7 times each concentration, obtaining 0.37%, 6.62%The analyte was monitored with an APCI source in negative ion mode to identify its fragments. The 24 analyzed samples presented PAT levels below the limit of quantification.A patulina (PAT) é uma micotoxina causada por certas espécies de fungos que, com certa frequência, contamina maçãs e produtos derivados, particularmente o suco. Esse contaminante tóxico é associado a efeitos mutagênicos, imunossupressivos e neurotóxicos em humanos e animais. No Brasil e no mundo o controle eficaz da contaminação por PAT depende de métodos analíticos confiáveis. Para um adequado monitoramento dos níveis de PAT em maçãs, é imprescindível utilizar processos que garantam um preparo adequado da amostra para a realização de uma análise cromatográfica correta. Este trabalho desenvolveu e validou uma técnica de análise de PAT em amostras de suco de maçã industrializado fundamentada na extração líquido-líquido, utilizando a acetonitrila como solvente extrator. A detecção por espectrometria de massas foi realizada após ionização química à pressão atmosférica (APCI). As recuperações médias alcançadas para as concentrações de 4, 8 e 20 μg/L de PAT foram de 97,5%, 92,49% e 96,92 %, respectivamente. A recuperação média do método foi de 95,64%. A reprodutibilidade da metodologia apresentada foi confirmada quando os resultados de um teste de proficiência de FAPAS, apresentando uma recuperação de 95,9%, além de apresentar uma boa seletividade. A incerteza do método foi estimada em três dias diferentes para três concentrações 4, 8 and 20 μg/L em replicatas de 7 vezes cada concentração, obtendo 0,37 %, 6,62 %. O analito foi monitorado por APCI no modo negativo para identificação de seus fragmentos. As 24 amostras de sucos de maçã analisadas apresentaram níveis de PAT abaixo do limite de quantificação.porUniversidade Federal de Santa MariaCentro de Ciências RuraisPrograma de Pós-Graduação em Medicina VeterináriaUFSMBrasilMedicina VeterináriaAttribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/info:eu-repo/semantics/openAccessMaçãMicotoxinasPatulinaExtraçãoLC-MS/MSAppleMycotoxinsPatulinExtractionLC-MS/MSValidationCNPQ::CIENCIAS AGRARIAS::MEDICINA VETERINARIAValidação e determinação de patulina em suco de maçã utilizando cromatografia líquida acoplada a espectrometria de massa tandemValidation and determination of patulin in apple juice using liquid chromatography and tandem mass spectrometryinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisMallmann, Carlos Augustohttp://lattes.cnpq.br/5193771213666058Vogel, Fernanda Silveira Flôreshttp://lattes.cnpq.br/9676833435314493Bairros, André Valle deTonini, CamilaSilva, Cristiane Rosa da500500000007600600600600600600f8b7bb02-50a2-468a-91b2-0a75e5374e2f7bab57c6-f800-4432-8837-8f4aacc2d40687a417ae-60eb-4318-9a6c-e38e8b3da5d629d69eb3-a890-4f52-ae8b-9c76411bcf35b5c499a2-10c5-4235-b247-07270efcf0b7reponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGMV_2021_SILVA_CRISTIANE.pdfDIS_PPGMV_2021_SILVA_CRISTIANE.pdfDissertação de Mestradoapplication/pdf1003485http://repositorio.ufsm.br/bitstream/1/22734/1/DIS_PPGMV_2021_SILVA_CRISTIANE.pdf29bb75bf2477fd7ebd203f7afca473baMD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Validação e determinação de patulina em suco de maçã utilizando cromatografia líquida acoplada a espectrometria de massa tandem |
dc.title.alternative.eng.fl_str_mv |
Validation and determination of patulin in apple juice using liquid chromatography and tandem mass spectrometry |
title |
Validação e determinação de patulina em suco de maçã utilizando cromatografia líquida acoplada a espectrometria de massa tandem |
spellingShingle |
Validação e determinação de patulina em suco de maçã utilizando cromatografia líquida acoplada a espectrometria de massa tandem Silva, Cristiane Rosa da Maçã Micotoxinas Patulina Extração LC-MS/MS Apple Mycotoxins Patulin Extraction LC-MS/MS Validation CNPQ::CIENCIAS AGRARIAS::MEDICINA VETERINARIA |
title_short |
Validação e determinação de patulina em suco de maçã utilizando cromatografia líquida acoplada a espectrometria de massa tandem |
title_full |
Validação e determinação de patulina em suco de maçã utilizando cromatografia líquida acoplada a espectrometria de massa tandem |
title_fullStr |
Validação e determinação de patulina em suco de maçã utilizando cromatografia líquida acoplada a espectrometria de massa tandem |
title_full_unstemmed |
Validação e determinação de patulina em suco de maçã utilizando cromatografia líquida acoplada a espectrometria de massa tandem |
title_sort |
Validação e determinação de patulina em suco de maçã utilizando cromatografia líquida acoplada a espectrometria de massa tandem |
author |
Silva, Cristiane Rosa da |
author_facet |
Silva, Cristiane Rosa da |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Mallmann, Carlos Augusto |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/5193771213666058 |
dc.contributor.advisor-co1.fl_str_mv |
Vogel, Fernanda Silveira Flôres |
dc.contributor.advisor-co1Lattes.fl_str_mv |
http://lattes.cnpq.br/9676833435314493 |
dc.contributor.referee1.fl_str_mv |
Bairros, André Valle de |
dc.contributor.referee2.fl_str_mv |
Tonini, Camila |
dc.contributor.author.fl_str_mv |
Silva, Cristiane Rosa da |
contributor_str_mv |
Mallmann, Carlos Augusto Vogel, Fernanda Silveira Flôres Bairros, André Valle de Tonini, Camila |
dc.subject.por.fl_str_mv |
Maçã Micotoxinas Patulina Extração LC-MS/MS |
topic |
Maçã Micotoxinas Patulina Extração LC-MS/MS Apple Mycotoxins Patulin Extraction LC-MS/MS Validation CNPQ::CIENCIAS AGRARIAS::MEDICINA VETERINARIA |
dc.subject.eng.fl_str_mv |
Apple Mycotoxins Patulin Extraction LC-MS/MS Validation |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS AGRARIAS::MEDICINA VETERINARIA |
description |
Patulin (PAT) is a mycotoxin produced by certain fungal species which is frequently found contaminating apples and derived products, especially juice. Several fungal pathogens, in particular Penicillium species, have been identified as causative agents of diseases in apples. PAT contamination may occur due to reasons as geographic differences, climatic conditions, agricultural practices, cultivars and postharvest environment, which may affect fruit composition. This toxic contaminant is associated with mutagenic, immunosuppressive and neurotoxic effects in humans and animals. In Brazil and in the world effective control of PAT contamination depends on reliable analytical methods. This study developed and validated a technique for the analysis of PAT in samples of industrialized apple juice based on liquid-liquid extraction, using acetonitrile as the extraction solvent. Detection via mass spectrometry was performed after Atmospher Pressure Chemical Ionization (APCI). Mean recoveries of 97.5, 92.49 and 96.92% were reached for 4, 8 and 20 μg/L of PAT, respectively. The mean recovery of the method was 95.64%. The reproducibility of the presented methodology was confirmed when the results of a FAPAS proficiency test, showing a 95.9% recovery, in addition to presenting a good selectivity. The method uncertainty was estimated on three different days for three concentrations 4, 8 and 20 μg / L in replicates of 7 times each concentration, obtaining 0.37%, 6.62%The analyte was monitored with an APCI source in negative ion mode to identify its fragments. The 24 analyzed samples presented PAT levels below the limit of quantification. |
publishDate |
2021 |
dc.date.accessioned.fl_str_mv |
2021-11-05T17:04:40Z |
dc.date.available.fl_str_mv |
2021-11-05T17:04:40Z |
dc.date.issued.fl_str_mv |
2021-03-04 |
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/1/22734 |
url |
http://repositorio.ufsm.br/handle/1/22734 |
dc.language.iso.fl_str_mv |
por |
language |
por |
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500500000007 |
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 Rurais |
dc.publisher.program.fl_str_mv |
Programa de Pós-Graduação em Medicina Veterinária |
dc.publisher.initials.fl_str_mv |
UFSM |
dc.publisher.country.fl_str_mv |
Brasil |
dc.publisher.department.fl_str_mv |
Medicina Veterinária |
publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Rurais |
dc.source.none.fl_str_mv |
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