Método multirresíduo para determinação de micotoxinas em vinho por UPLC-MS/MS
Ano de defesa: | 2013 |
---|---|
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
|
Programa de Pós-Graduação: |
Programa de Pós-Graduação em Química
|
Departamento: |
Química
|
País: |
BR
|
Palavras-chave em Português: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/10533 |
Resumo: | A fast multimethod using liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was implemented and optimized to yield a complete determination of 36 mycotoxins in wine samples. Extraction was performed with acetonitrile, applying modified QuEChERS method (Quick, Easy, Cheap, Effective, Rugged and Safe). Traditionally, QuEChERS method is well known in pesticides determination in a variety of matrices and due this has received the distinction of an AOAC (Association of Official Agricultural Chemists) official method for multiple pesticides in fruits and vegetables (LEHOTAY et al., 2005; BANERJEE et al., 2009). Usually mycotoxins analysis are carried out by liquid chromatography after immunoaffinity column clean-up or by enzyme-linked immunosorbent assay tests, but all these methods normally involve determination of a single compounds only (SPANJER et al., 2008; CUNHA et al., 2009). This study aimed to apply modified QuEChERS method as extraction procedure for mycotoxins determination in wine samples.During this study, were performed optimization experiments to improve recovery results and analites stability. Besides the evaluation of the proper volume of wine samples to be applied, tests were performed to test pH effect by using an additional buffering step with ammonium formate/ formic acid. Normally this method apply a dispersive clean-up with sorbents to clean-up sample extract. This procedure followed a dSPE clean-up with various sorbents where mycotoxins were analyzed on UPLC-MS/MS system, using electrospray ionization in positive mode. Mycotoxins standards stock solutions were prepared and classified in three different groups, with different range of concentration. Recovery studies were performed by analyzing samples in three spiked levels, with six (n=6) replicates in each concentration. Other validation parameters evaluated were linearity (r2) of calibration curves, accuracy (recovery %), instrument limits of detection and method limits of quantification (LOD and LOQ), precision (RSD%) and matrix effects (%) were determined for each individual mycotoxin. From 36 mycotoxins analyzed by UPLC-MS/MS (ESI+), 35 showed average recoveries between 70-120% and 88% an RSD ≤ 20%, at the lowest spiked level (Group I = 1, Group II = 50 e Group III = 10 μg kg-1). The method LOQ for 86% mycotoxins was the lowest level studied. The observed matrix effect was lower than ±20% for 75% of mycotoxins. This procedure was applied successfully also in a survey of 56 red wine samples purchased in the city of Amsterdam (The Netherlands) from many different countries. |
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2017-05-182017-05-182013-01-08RIGHI, Laís Weber. Multiresidue method for the uplc-ms/ms analysis of mycotoxins in wine. 2013. 142 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013.http://repositorio.ufsm.br/handle/1/10533A fast multimethod using liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was implemented and optimized to yield a complete determination of 36 mycotoxins in wine samples. Extraction was performed with acetonitrile, applying modified QuEChERS method (Quick, Easy, Cheap, Effective, Rugged and Safe). Traditionally, QuEChERS method is well known in pesticides determination in a variety of matrices and due this has received the distinction of an AOAC (Association of Official Agricultural Chemists) official method for multiple pesticides in fruits and vegetables (LEHOTAY et al., 2005; BANERJEE et al., 2009). Usually mycotoxins analysis are carried out by liquid chromatography after immunoaffinity column clean-up or by enzyme-linked immunosorbent assay tests, but all these methods normally involve determination of a single compounds only (SPANJER et al., 2008; CUNHA et al., 2009). This study aimed to apply modified QuEChERS method as extraction procedure for mycotoxins determination in wine samples.During this study, were performed optimization experiments to improve recovery results and analites stability. Besides the evaluation of the proper volume of wine samples to be applied, tests were performed to test pH effect by using an additional buffering step with ammonium formate/ formic acid. Normally this method apply a dispersive clean-up with sorbents to clean-up sample extract. This procedure followed a dSPE clean-up with various sorbents where mycotoxins were analyzed on UPLC-MS/MS system, using electrospray ionization in positive mode. Mycotoxins standards stock solutions were prepared and classified in three different groups, with different range of concentration. Recovery studies were performed by analyzing samples in three spiked levels, with six (n=6) replicates in each concentration. Other validation parameters evaluated were linearity (r2) of calibration curves, accuracy (recovery %), instrument limits of detection and method limits of quantification (LOD and LOQ), precision (RSD%) and matrix effects (%) were determined for each individual mycotoxin. From 36 mycotoxins analyzed by UPLC-MS/MS (ESI+), 35 showed average recoveries between 70-120% and 88% an RSD ≤ 20%, at the lowest spiked level (Group I = 1, Group II = 50 e Group III = 10 μg kg-1). The method LOQ for 86% mycotoxins was the lowest level studied. The observed matrix effect was lower than ±20% for 75% of mycotoxins. This procedure was applied successfully also in a survey of 56 red wine samples purchased in the city of Amsterdam (The Netherlands) from many different countries.Um método rápido usando cromatografia líquida de ultra eficiência acoplada a espectrometria de massas (UPLC-MS/MS) foi implementado e otimizado para proporcionar a determinação completa de 36 micotoxinas em amostras de vinhos. A extração foi realizada com acetonitrila, aplicando o método QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe; em português: Rápido, Fácil, Barato, Efetivo, Robusto e Seguro) modificado. Tradicionalmente, o método QuEChERS é muito conhecido na determinação de múltiplos pesticidas em uma grande variedade de matrizes de frutas e vegetais e por essa razão recebeu a distinção de método oficial da AOAC (Association of Official Agricultural Chemists) (LEHOTAY et al., 2005; BANERJEE et al., 2009). Normalmente, as determinações de micotoxinas são realizadas por cromatografia líquida após purificação em coluna de imunoafinidade ou testes ELISA, porém, essas técnicas possuem a desvantagem de envolver a determinação individual dos analitos (SPANJER et al., 2008; CUNHA et al., 2009). O objetivo deste estudo foi otimizar e empregar o método QuEChERS no procedimento de extração para determinação de micotoxinas em amostras de vinho. Durante o estudo, foram realizados experimentos de otimização para melhorar a recuperação e estabilidade dos analitos. Além da avaliação do volume da amostra de vinho tinto a ser empregado, foi estudado o efeito do pH, realizado pela adição de uma etapa de tamponamento com formiato de amônio e ácido fórmico. Esse método envolveu uma etapa de purificação do extrato por dSPE, avaliando o uso de vários adsorventes. As micotoxinas foram analisadas por UPLC-MS/MS, usando ionização por eletronebulização no modo positivo. As soluções padrão de micotoxinas foram preparadas e classificadas em três diferentes grupos, com faixas de concentração diferentes. O estudo de recuperação foi realizado em três diferentes níveis de fortificação, com seis replicatas (n=6) em cada concentração. Outros parâmetros avaliados da validação foram linearidade (r2) das curvas analíticas, exatidão (% de recuperação), limites de detecção e de quantificação do método (LOQ e LOD, respectivamente), precisão (RSD%) e efeito matriz (%), determinados individualmente para cada micotoxina. Das 36 micotoxinas analisadas por UPLC-MS/MS (ESI+), 35 apresentaram recuperação percentual entre 70-120% e 88% apresentaram RSD ≤ 20% no menor nível de fortificação estudado (Grupo I = 1, Grupo II = 50 e Grupo III = 10 μg kg-1). O LOQ do método para 86% das micotoxinas foi o nível mais baixo estudado. O efeito matriz observado foi inferior a ±20% para 75% das micotoxinas. Este método foi aplicado satisfatoriamente na análise de 56 amostras de vinho tinto adquiridos na cidade de Amsterdã (Holanda), provenientes de diversos países.Conselho Nacional de Desenvolvimento Científico e Tecnológicoapplication/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em QuímicaUFSMBRQuímicaQuímicaMicotoxinasVinhoCromatografia líquidaValidaçãoQuímica analíticaCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAMétodo multirresíduo para determinação de micotoxinas em vinho por UPLC-MS/MSMultiresidue method for the uplc-ms/ms analysis of mycotoxins in wineinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisPizzutti, Ionara Reginahttp://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4797011T5Jabor, Valquíria Aparecida Poliselhttp://lattes.cnpq.br/0210528747723945Gebler, Lucianohttp://lattes.cnpq.br/3800729962480769http://lattes.cnpq.br/3148033402810489Righi, Laís Weber100600000000400300300300300961b4a4a-1465-4d87-b4e8-6428b5a3ad389414d884-9abb-4a70-af49-9331c56db961c206dd7c-aece-4e55-b567-8b8469652b7e8e5b76c8-7237-49b4-9a3b-1ad829f79dd5info:eu-repo/semantics/openAccessreponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALRIGHI, LAIS WEBER.pdfapplication/pdf2215731http://repositorio.ufsm.br/bitstream/1/10533/1/RIGHI%2c%20LAIS%20WEBER.pdf8abdd008d55646e4c50e0073e9c85f6eMD51TEXTRIGHI, LAIS WEBER.pdf.txtRIGHI, LAIS WEBER.pdf.txtExtracted texttext/plain212135http://repositorio.ufsm.br/bitstream/1/10533/2/RIGHI%2c%20LAIS%20WEBER.pdf.txt9aa048f4e1a2d6c19179d6b7fbb009a1MD52THUMBNAILRIGHI, LAIS WEBER.pdf.jpgRIGHI, LAIS WEBER.pdf.jpgIM Thumbnailimage/jpeg4552http://repositorio.ufsm.br/bitstream/1/10533/3/RIGHI%2c%20LAIS%20WEBER.pdf.jpg3ba1eda5e360265d6df99989bac4ee30MD531/105332017-07-25 12:05:15.942oai:repositorio.ufsm.br:1/10533Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2017-07-25T15:05:15Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Método multirresíduo para determinação de micotoxinas em vinho por UPLC-MS/MS |
dc.title.alternative.eng.fl_str_mv |
Multiresidue method for the uplc-ms/ms analysis of mycotoxins in wine |
title |
Método multirresíduo para determinação de micotoxinas em vinho por UPLC-MS/MS |
spellingShingle |
Método multirresíduo para determinação de micotoxinas em vinho por UPLC-MS/MS Righi, Laís Weber Química Micotoxinas Vinho Cromatografia líquida Validação Química analítica CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Método multirresíduo para determinação de micotoxinas em vinho por UPLC-MS/MS |
title_full |
Método multirresíduo para determinação de micotoxinas em vinho por UPLC-MS/MS |
title_fullStr |
Método multirresíduo para determinação de micotoxinas em vinho por UPLC-MS/MS |
title_full_unstemmed |
Método multirresíduo para determinação de micotoxinas em vinho por UPLC-MS/MS |
title_sort |
Método multirresíduo para determinação de micotoxinas em vinho por UPLC-MS/MS |
author |
Righi, Laís Weber |
author_facet |
Righi, Laís Weber |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Pizzutti, Ionara Regina |
dc.contributor.advisor1Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4797011T5 |
dc.contributor.referee1.fl_str_mv |
Jabor, Valquíria Aparecida Polisel |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/0210528747723945 |
dc.contributor.referee2.fl_str_mv |
Gebler, Luciano |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/3800729962480769 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/3148033402810489 |
dc.contributor.author.fl_str_mv |
Righi, Laís Weber |
contributor_str_mv |
Pizzutti, Ionara Regina Jabor, Valquíria Aparecida Polisel Gebler, Luciano |
dc.subject.por.fl_str_mv |
Química Micotoxinas Vinho Cromatografia líquida Validação Química analítica |
topic |
Química Micotoxinas Vinho Cromatografia líquida Validação Química analítica CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
A fast multimethod using liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was implemented and optimized to yield a complete determination of 36 mycotoxins in wine samples. Extraction was performed with acetonitrile, applying modified QuEChERS method (Quick, Easy, Cheap, Effective, Rugged and Safe). Traditionally, QuEChERS method is well known in pesticides determination in a variety of matrices and due this has received the distinction of an AOAC (Association of Official Agricultural Chemists) official method for multiple pesticides in fruits and vegetables (LEHOTAY et al., 2005; BANERJEE et al., 2009). Usually mycotoxins analysis are carried out by liquid chromatography after immunoaffinity column clean-up or by enzyme-linked immunosorbent assay tests, but all these methods normally involve determination of a single compounds only (SPANJER et al., 2008; CUNHA et al., 2009). This study aimed to apply modified QuEChERS method as extraction procedure for mycotoxins determination in wine samples.During this study, were performed optimization experiments to improve recovery results and analites stability. Besides the evaluation of the proper volume of wine samples to be applied, tests were performed to test pH effect by using an additional buffering step with ammonium formate/ formic acid. Normally this method apply a dispersive clean-up with sorbents to clean-up sample extract. This procedure followed a dSPE clean-up with various sorbents where mycotoxins were analyzed on UPLC-MS/MS system, using electrospray ionization in positive mode. Mycotoxins standards stock solutions were prepared and classified in three different groups, with different range of concentration. Recovery studies were performed by analyzing samples in three spiked levels, with six (n=6) replicates in each concentration. Other validation parameters evaluated were linearity (r2) of calibration curves, accuracy (recovery %), instrument limits of detection and method limits of quantification (LOD and LOQ), precision (RSD%) and matrix effects (%) were determined for each individual mycotoxin. From 36 mycotoxins analyzed by UPLC-MS/MS (ESI+), 35 showed average recoveries between 70-120% and 88% an RSD ≤ 20%, at the lowest spiked level (Group I = 1, Group II = 50 e Group III = 10 μg kg-1). The method LOQ for 86% mycotoxins was the lowest level studied. The observed matrix effect was lower than ±20% for 75% of mycotoxins. This procedure was applied successfully also in a survey of 56 red wine samples purchased in the city of Amsterdam (The Netherlands) from many different countries. |
publishDate |
2013 |
dc.date.issued.fl_str_mv |
2013-01-08 |
dc.date.accessioned.fl_str_mv |
2017-05-18 |
dc.date.available.fl_str_mv |
2017-05-18 |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/masterThesis |
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masterThesis |
status_str |
publishedVersion |
dc.identifier.citation.fl_str_mv |
RIGHI, Laís Weber. Multiresidue method for the uplc-ms/ms analysis of mycotoxins in wine. 2013. 142 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013. |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/10533 |
identifier_str_mv |
RIGHI, Laís Weber. Multiresidue method for the uplc-ms/ms analysis of mycotoxins in wine. 2013. 142 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2013. |
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http://repositorio.ufsm.br/handle/1/10533 |
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