Validação e determinação de patulina em suco de maçã utilizando cromatografia líquida acoplada a espectrometria de massa tandem

Detalhes bibliográficos
Autor(a) principal: Silva, Cristiane Rosa da
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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spelling 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
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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
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