Determinação simultânea de agrotóxicos e micotoxinas em fitoterápicos: Validação e aplicação de métodos multirresíduo empregando LC-MS/MS
Autor(a) principal: | |
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Data de Publicação: | 2023 |
Tipo de documento: | Tese |
Idioma: | por |
Título da fonte: | Manancial - Repositório Digital da UFSM |
Texto Completo: | http://repositorio.ufsm.br/handle/1/31548 |
Resumo: | The use of herbal medicines has increased significantly, but the presence of pesticide residues as well as the presence of mycotoxins have generated constant discussion and concern on the part of regulatory agencies. The development of analytical methods for the determination of pesticides and mycotoxins in medicinal plants is a great challenge, due to the substances naturally present in plants. In this study, QuEChERS was optimized followed by analysis by liquid chromatography coupled with sequential mass spectrometry for simultaneous determination of pesticides and mycotoxins in Melissa officinalis and Malva Sylvestris. The final method was validated according to SANTE/11312/2021 and consists of a variation of the QuEChERS method. In a 50 mL Falcon tube, 12 and 14 g of slurry were weighed. Then, 10 mL of acetonitrile 1% formic acid (v/v) containing the procedure's internal standard were added. The tubes were shaken on a mechanical shaker for 1 min. Then, 4 g of magnesium sulfate and 1 g of sodium chloride were added, and the samples were shaken again for 1 minute. The extracts were centrifuged, and 1 mL of the supernatant was quantitatively transferred to a dispersive clean-up kit containing a mixture of 25 mg PSA, 7.5 mg GCB and 150 mg MgSO4. The tubes were homogenized in vortex for 1 min and centrifuged again and 0.5 mL of extract was transferred to a vial and diluted with 0.5 mL of acetonitrile/water (1:1, v/v) containing the instrument's internal standard. The quantification limit ranged from 2 to 500 μg kg-1. Although some analytes still exhibited analytical signal suppression due to considerable matrix effect, an adequate linear range for matrix-paired calibration standards was achieved with adequate method performance due to the resolution of the mass spectrometer used. In all, 146 pesticides and 11 mycotoxins were validated for Melissa officinalis and 144 and 9 for Malva sylvestris. Commercial samples were analyzed and no residue above the detection limit was found, showing the quality of products marketed in the state of Rio Grande do Sul. |
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Determinação simultânea de agrotóxicos e micotoxinas em fitoterápicos: Validação e aplicação de métodos multirresíduo empregando LC-MS/MSSimultaneous determination of pesticides and mycotoxins in herbal medicines: validation and application of a multiresidue method using LC-MS/MSFitoterápicosMicotoxinasAgrotóxicosCromatografia líquidaEspectrometria de massasMedicinal herbsMycotoxinsPesticidesLiquid chromatographyMass spectrometryCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAThe use of herbal medicines has increased significantly, but the presence of pesticide residues as well as the presence of mycotoxins have generated constant discussion and concern on the part of regulatory agencies. The development of analytical methods for the determination of pesticides and mycotoxins in medicinal plants is a great challenge, due to the substances naturally present in plants. In this study, QuEChERS was optimized followed by analysis by liquid chromatography coupled with sequential mass spectrometry for simultaneous determination of pesticides and mycotoxins in Melissa officinalis and Malva Sylvestris. The final method was validated according to SANTE/11312/2021 and consists of a variation of the QuEChERS method. In a 50 mL Falcon tube, 12 and 14 g of slurry were weighed. Then, 10 mL of acetonitrile 1% formic acid (v/v) containing the procedure's internal standard were added. The tubes were shaken on a mechanical shaker for 1 min. Then, 4 g of magnesium sulfate and 1 g of sodium chloride were added, and the samples were shaken again for 1 minute. The extracts were centrifuged, and 1 mL of the supernatant was quantitatively transferred to a dispersive clean-up kit containing a mixture of 25 mg PSA, 7.5 mg GCB and 150 mg MgSO4. The tubes were homogenized in vortex for 1 min and centrifuged again and 0.5 mL of extract was transferred to a vial and diluted with 0.5 mL of acetonitrile/water (1:1, v/v) containing the instrument's internal standard. The quantification limit ranged from 2 to 500 μg kg-1. Although some analytes still exhibited analytical signal suppression due to considerable matrix effect, an adequate linear range for matrix-paired calibration standards was achieved with adequate method performance due to the resolution of the mass spectrometer used. In all, 146 pesticides and 11 mycotoxins were validated for Melissa officinalis and 144 and 9 for Malva sylvestris. Commercial samples were analyzed and no residue above the detection limit was found, showing the quality of products marketed in the state of Rio Grande do Sul.O uso de fitoterápicos tem aumentado expressivamente, porém a possível presença de resíduos de agrotóxicos bem como de micotoxinas têm gerado constante discussão e preocupação por parte dos órgãos reguladores. O desenvolvimento de métodos analíticos para determinação de agrotóxicos e micotoxinas em plantas medicinais é um grande desafio, devido às substâncias naturalmente presentes nestas matrizes. Neste estudo, foi otimizado o método QuEChERS seguida de análise por cromatografia liquida acoplada a espectrometria de massas sequencial para determinação simultânea de agrotóxicos e micotoxinas em Melissa officinalis e Malva Sylvestris. O método final foi validado de acordo com o SANTE/11312/2021 e consiste em uma variação do método QuEChERS. Foram pesados 12 e 14 g de slurry. Em seguida, foram adicionados 10 mL de acetonitrila 1% ácido fórmico (v/v) contendo do padrão interno do procedimento. Os tubos foram agitados em agitador mecânico por 1 min. Em seguida, adicionaram-se 4 g de sulfato de magnésio e 1 g de cloreto de sódio e as amostras foram agitadas novamente por 1 min. Os extratos foram centrifugados e 1 mL do sobrenadante foi transferido quantitativamente para um kit de clean-up dispersivo contendo uma mistura de 25 mg de PSA, 7,5 mg de GCB e 150 mg de MgSO4. Os tubos foram homogeneizados em vórtex por 1 min e novamente centrifugados onde 0,5 mL de extrato foi transferido para um vial e diluído com 0,5 mL de acetonitrila/água (1:1, v/v) contendo padrão interno do instrumento. O limite de quantificação variou na faixa de 2 a 500 μg kg-1. Embora alguns analitos ainda apresentassem uma supressão de sinal analítico devido a um efeito de matriz considerável, uma faixa linear adequada para padrões de calibração pareados por matriz foi alcançada com desempenho de método adequado devido à resolução do espectrômetro de massas empregado. Ao todo, os métodos multirresíduos foram validades para determinação de146 agrotóxicos e 11 micotoxinas para Melissa officinalis e 144 agrotóxicos e 9 micotoxinas para Malva sylvestris. Amostras comerciais foram analisadas e nenhum resíduo das substâncias estudadas foi maior do que o limite de detecção mostrando a qualidade dos produtos comercializados no estado do Rio Grande do Sul.Universidade Federal de Santa MariaBrasilQuímicaUFSMPrograma de Pós-Graduação em QuímicaCentro de Ciências Naturais e ExatasPizzutti, Ionara Reginahttp://lattes.cnpq.br/3883506164936996Dias, Jonatan ViniciusRosa, Marcelo Barcellos daHoffmann, Jessica FernandaSilva, Rosselei Caiel daFontana, Marlos Eduardo Zorzella2024-02-21T11:01:46Z2024-02-21T11:01:46Z2023-02-27info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisapplication/pdfhttp://repositorio.ufsm.br/handle/1/31548porAttribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/info:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSM2024-02-21T11:01:46Zoai:repositorio.ufsm.br:1/31548Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2024-02-21T11:01:46Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.none.fl_str_mv |
Determinação simultânea de agrotóxicos e micotoxinas em fitoterápicos: Validação e aplicação de métodos multirresíduo empregando LC-MS/MS Simultaneous determination of pesticides and mycotoxins in herbal medicines: validation and application of a multiresidue method using LC-MS/MS |
title |
Determinação simultânea de agrotóxicos e micotoxinas em fitoterápicos: Validação e aplicação de métodos multirresíduo empregando LC-MS/MS |
spellingShingle |
Determinação simultânea de agrotóxicos e micotoxinas em fitoterápicos: Validação e aplicação de métodos multirresíduo empregando LC-MS/MS Fontana, Marlos Eduardo Zorzella Fitoterápicos Micotoxinas Agrotóxicos Cromatografia líquida Espectrometria de massas Medicinal herbs Mycotoxins Pesticides Liquid chromatography Mass spectrometry CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação simultânea de agrotóxicos e micotoxinas em fitoterápicos: Validação e aplicação de métodos multirresíduo empregando LC-MS/MS |
title_full |
Determinação simultânea de agrotóxicos e micotoxinas em fitoterápicos: Validação e aplicação de métodos multirresíduo empregando LC-MS/MS |
title_fullStr |
Determinação simultânea de agrotóxicos e micotoxinas em fitoterápicos: Validação e aplicação de métodos multirresíduo empregando LC-MS/MS |
title_full_unstemmed |
Determinação simultânea de agrotóxicos e micotoxinas em fitoterápicos: Validação e aplicação de métodos multirresíduo empregando LC-MS/MS |
title_sort |
Determinação simultânea de agrotóxicos e micotoxinas em fitoterápicos: Validação e aplicação de métodos multirresíduo empregando LC-MS/MS |
author |
Fontana, Marlos Eduardo Zorzella |
author_facet |
Fontana, Marlos Eduardo Zorzella |
author_role |
author |
dc.contributor.none.fl_str_mv |
Pizzutti, Ionara Regina http://lattes.cnpq.br/3883506164936996 Dias, Jonatan Vinicius Rosa, Marcelo Barcellos da Hoffmann, Jessica Fernanda Silva, Rosselei Caiel da |
dc.contributor.author.fl_str_mv |
Fontana, Marlos Eduardo Zorzella |
dc.subject.por.fl_str_mv |
Fitoterápicos Micotoxinas Agrotóxicos Cromatografia líquida Espectrometria de massas Medicinal herbs Mycotoxins Pesticides Liquid chromatography Mass spectrometry CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
topic |
Fitoterápicos Micotoxinas Agrotóxicos Cromatografia líquida Espectrometria de massas Medicinal herbs Mycotoxins Pesticides Liquid chromatography Mass spectrometry CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
The use of herbal medicines has increased significantly, but the presence of pesticide residues as well as the presence of mycotoxins have generated constant discussion and concern on the part of regulatory agencies. The development of analytical methods for the determination of pesticides and mycotoxins in medicinal plants is a great challenge, due to the substances naturally present in plants. In this study, QuEChERS was optimized followed by analysis by liquid chromatography coupled with sequential mass spectrometry for simultaneous determination of pesticides and mycotoxins in Melissa officinalis and Malva Sylvestris. The final method was validated according to SANTE/11312/2021 and consists of a variation of the QuEChERS method. In a 50 mL Falcon tube, 12 and 14 g of slurry were weighed. Then, 10 mL of acetonitrile 1% formic acid (v/v) containing the procedure's internal standard were added. The tubes were shaken on a mechanical shaker for 1 min. Then, 4 g of magnesium sulfate and 1 g of sodium chloride were added, and the samples were shaken again for 1 minute. The extracts were centrifuged, and 1 mL of the supernatant was quantitatively transferred to a dispersive clean-up kit containing a mixture of 25 mg PSA, 7.5 mg GCB and 150 mg MgSO4. The tubes were homogenized in vortex for 1 min and centrifuged again and 0.5 mL of extract was transferred to a vial and diluted with 0.5 mL of acetonitrile/water (1:1, v/v) containing the instrument's internal standard. The quantification limit ranged from 2 to 500 μg kg-1. Although some analytes still exhibited analytical signal suppression due to considerable matrix effect, an adequate linear range for matrix-paired calibration standards was achieved with adequate method performance due to the resolution of the mass spectrometer used. In all, 146 pesticides and 11 mycotoxins were validated for Melissa officinalis and 144 and 9 for Malva sylvestris. Commercial samples were analyzed and no residue above the detection limit was found, showing the quality of products marketed in the state of Rio Grande do Sul. |
publishDate |
2023 |
dc.date.none.fl_str_mv |
2023-02-27 2024-02-21T11:01:46Z 2024-02-21T11:01:46Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/doctoralThesis |
format |
doctoralThesis |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/31548 |
url |
http://repositorio.ufsm.br/handle/1/31548 |
dc.language.iso.fl_str_mv |
por |
language |
por |
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.format.none.fl_str_mv |
application/pdf |
dc.publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Brasil Química UFSM Programa de Pós-Graduação em Química Centro de Ciências Naturais e Exatas |
publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Brasil Química UFSM Programa de Pós-Graduação em Química Centro de Ciências Naturais e Exatas |
dc.source.none.fl_str_mv |
reponame:Manancial - Repositório Digital da UFSM instname:Universidade Federal de Santa Maria (UFSM) instacron:UFSM |
instname_str |
Universidade Federal de Santa Maria (UFSM) |
instacron_str |
UFSM |
institution |
UFSM |
reponame_str |
Manancial - Repositório Digital da UFSM |
collection |
Manancial - Repositório Digital da UFSM |
repository.name.fl_str_mv |
Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
atendimento.sib@ufsm.br||tedebc@gmail.com |
_version_ |
1805922165391884288 |