Determinação multiclasse de resíduos de agrotóxicos e medicamentos veterinários em carnes por LC-MS/MS
Ano de defesa: | 2012 |
---|---|
Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | , , |
Tipo de documento: | Tese |
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: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/4219 |
Resumo: | The agribusiness has been incorporating new technologies in the production of meat, including good management of farms, health, balanced diet, breeding and integrated production. Allied to this, there is a growing concern with issues related to residues and contaminants in animals intended for food production. In the study, were compared four extraction methods based on the method QuEChERS for the determination of 79 pesticides and 15 veterinary drugs analyzed by Liquid Chromatography coupled to tandem Mass Spectrometry in samples of meat and pork liver, chicken and fish. The parameters evaluated were: linear range (6 concentration levels and 6 injections each), limit of detection (LOD), limit of quantification (LOQ), decision limit (CCα), capability of detection (CCβ) and matrix effect, as well as precision and accuracy, in terms of recovery. For this, we performed the fortification of matrices previously homogenized with solutions containing compounds at 3 levels of fortification (20, 50 and 100 μg kg-1), 6 replicates for each level, were performade. The modified QuEChERS extraction method consists in the extraction of 10 g of the matrix with 10 mL of acetonitrile containing 1% (v/v) of acetic acid and shaking vigorously by hand for 1 min. After, 4 g of anhydrous magnesium sulfate and 1.7 g anhydrous sodium acetate were added and the agitation repeated. After the extract was centrifugated for 8 min (3500 rpm) and 2 mL of the extract was transferred to another tube containing 300 mg of anhydrous magnesium sulfate and 50 mg of sorbent PSA, repeating the agitation and centrifugation. The extract was diluted (1:1 v/v) in the mobile phase and then analyzed by LC-MS/MS. Analytical curves prepared in solvent and in extracts of matrices evaluated showed adequate linearity between 5 and 200 μg kg-1, with coefficients of determination greater than 0.99. The method showed satisfactory recovery values between 70 and 120% (RSD ≤ 20%) to about 95% of compounds in all matrices, except for liver showed satisfactory values to about 80% of the compound at levels of 20, 50 and 100 μg kg-1. The LOQ of method was 10 μg kg-1. CCα values were between 1.1 and 102.9 μg kg-1 and CCβ values were in the range 1.9 to 105.9 μg kg-1. The results of this study showed that the modified method QuEChERS is fast, simple and efficient and can be applied to the determination of pesticides and veterinary drugs in samples of meat and liver pork, chicken and fish fillet for routine analysis. Furthermore, the use of LC-MS/MS was efficent, allowing the determination and confirmation of a large number of compounds simultaneously at residues livels. |
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2017-05-112017-05-112012-03-23FRIGGI, Caroline do Amaral. Multiclass determination of pesticides and veterinary drugs residues in meat by LC-MS/MS. 2012. 151 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2012.http://repositorio.ufsm.br/handle/1/4219The agribusiness has been incorporating new technologies in the production of meat, including good management of farms, health, balanced diet, breeding and integrated production. Allied to this, there is a growing concern with issues related to residues and contaminants in animals intended for food production. In the study, were compared four extraction methods based on the method QuEChERS for the determination of 79 pesticides and 15 veterinary drugs analyzed by Liquid Chromatography coupled to tandem Mass Spectrometry in samples of meat and pork liver, chicken and fish. The parameters evaluated were: linear range (6 concentration levels and 6 injections each), limit of detection (LOD), limit of quantification (LOQ), decision limit (CCα), capability of detection (CCβ) and matrix effect, as well as precision and accuracy, in terms of recovery. For this, we performed the fortification of matrices previously homogenized with solutions containing compounds at 3 levels of fortification (20, 50 and 100 μg kg-1), 6 replicates for each level, were performade. The modified QuEChERS extraction method consists in the extraction of 10 g of the matrix with 10 mL of acetonitrile containing 1% (v/v) of acetic acid and shaking vigorously by hand for 1 min. After, 4 g of anhydrous magnesium sulfate and 1.7 g anhydrous sodium acetate were added and the agitation repeated. After the extract was centrifugated for 8 min (3500 rpm) and 2 mL of the extract was transferred to another tube containing 300 mg of anhydrous magnesium sulfate and 50 mg of sorbent PSA, repeating the agitation and centrifugation. The extract was diluted (1:1 v/v) in the mobile phase and then analyzed by LC-MS/MS. Analytical curves prepared in solvent and in extracts of matrices evaluated showed adequate linearity between 5 and 200 μg kg-1, with coefficients of determination greater than 0.99. The method showed satisfactory recovery values between 70 and 120% (RSD ≤ 20%) to about 95% of compounds in all matrices, except for liver showed satisfactory values to about 80% of the compound at levels of 20, 50 and 100 μg kg-1. The LOQ of method was 10 μg kg-1. CCα values were between 1.1 and 102.9 μg kg-1 and CCβ values were in the range 1.9 to 105.9 μg kg-1. The results of this study showed that the modified method QuEChERS is fast, simple and efficient and can be applied to the determination of pesticides and veterinary drugs in samples of meat and liver pork, chicken and fish fillet for routine analysis. Furthermore, the use of LC-MS/MS was efficent, allowing the determination and confirmation of a large number of compounds simultaneously at residues livels.O agronegócio nacional vem incorporando novas tecnologias na produção de carnes, incluindo bom manejo das granjas, sanidade, alimentação balanceada, melhoramento genético e produção integrada. Aliado a este fato, há uma preocupação crescente com questões relacionadas à presença de resíduos e contaminantes em animais destinados a produção de alimentos. Neste estudo, comparou-se quatro métodos de extração baseados no método QuEChERS para a determinação de 79 agrotóxicos e 15 medicamentos veterinários por Cromatografia Líquida acoplada à Espectrometria de Massas em Série em amostras de carne e fígado suíno, carne de frango e filé de peixe. Os parâmetros avaliados foram: faixa de linear das curvas analíticas (6 níveis de concentração e 6 injeções cada), limite de detecção (LOD), limite de quantificação (LOQ), limite de decisão (CCα), capacidade de detecção (CCβ) e efeito matriz, bem como precisão e exatidão, em termos de recuperação. Para isso, efetuou-se a fortificação das matrizes previamente homogeneizadas, com soluções contendo os compostos em 3 níveis de fortificação (20, 50 e 100 μg kg-1), 6 réplicas para cada nível, e aplicou-se o método proposto. A extração pelo método QuEChERS modificado consistiu na extração de 10,0 g da matriz com 10 mL de acetonitrila contendo 1% (v/v) de ácido acético sob agitação manual e vigorosa por 1 min. Acrescentou-se 4,0 g de sulfato de magnésio anidro e 1,7 g de acetato de sódio anidro, repetindo-se a agitação. O extrato foi centrifugado por 8 min (3500 rpm) e após 2 mL de extrato foram transferidos para outro tubo contendo 300 mg de sulfato de magnésio anidro e 50 mg de sorvente PSA, repetindo-se a agitação e a centrifugação. O extrato foi diluído (1:1) na fase móvel e em seguida analisado por LC-MS/MS. As curvas analíticas, preparadas no solvente e nos extratos das matrizes avaliadas, apresentaram linearidade adequada entre 5 e 200 μg L-1, com valores de coeficiente de determinação maiores que 0,99. O método apresentou valores de recuperação satisfatórios entre 70 e 120% e (RSD ≤ 20%) para cerca de 95% dos compostos em todas as matrizes, exceto para fígado que apresentou valores satisfatórios para cerca de 80% dos compostos nos níveis de 20, 50 e 100 μg kg-1. O valor de LOQ do método foi de 10 μg kg-1. Os valores de CCα ficaram entre 1,1 e 102,9 μg kg-1 e os valores de CCβ ficaram na faixa de 1,9 a 105,9 μg kg-1. Os resultados desse estudo mostraram que o método QuEChERS modificado é rápido, simples e eficiente, podendo ser aplicado para a determinação de agrotóxicos e medicamentos veterinários em amostras de carne e fígado suíno, carne de frango e filé de peixe em análise de rotina. Além disso, o emprego da LC-MS/MS mostrou-se eficiente, permitindo a determinação e confirmação de um grande número de compostos simultaneamente em níveis de resíduos.Coordenação de Aperfeiçoamento de Pessoal de Nível Superiorapplication/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em QuímicaUFSMBRQuímicaCarnesAgrotóxicosMedicamentos veterináriosQuEChERSLCMS/MSMeatPesticidesVeterinary drugsCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADeterminação multiclasse de resíduos de agrotóxicos e medicamentos veterinários em carnes por LC-MS/MSMulticlass determination of pesticides and veterinary drugs residues in meat by LC-MS/MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisZanella, Renatohttp://lattes.cnpq.br/2541865299438479Adaime, Martha Bohrerhttp://lattes.cnpq.br/4385786922516848Rath, Susannehttp://lattes.cnpq.br/4317826174161775Prestes, Osmar Damianhttp://lattes.cnpq.br/9632234955509028Richards, Neila Silvia Pereira dos Santoshttp://lattes.cnpq.br/0618653776990780http://lattes.cnpq.br/8099993750354618Friggi, Caroline do Amaral1006000000004003003003003003005000aa2baab-94e8-4d3d-bbb2-85495ba77db5ee70933c-ddf1-4a31-bc29-ac954a4aa1cee3f47b1c-bced-4ba5-a0c9-4d0204119f856886e7ee-1f53-4393-820d-930ef025c6344eef7b33-113c-470f-8729-f99c250df0281d335958-8f1e-4c60-b406-e90c5768a1b7info:eu-repo/semantics/openAccessreponame:Biblioteca Digital de Teses e Dissertações do UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALFRIGGI, CAROLINE DO AMARAL.pdfapplication/pdf4658394http://repositorio.ufsm.br/bitstream/1/4219/1/FRIGGI%2c%20CAROLINE%20DO%20AMARAL.pdf898858cbda8cafdb3d3912d5c6199816MD51TEXTFRIGGI, CAROLINE DO AMARAL.pdf.txtFRIGGI, CAROLINE DO AMARAL.pdf.txtExtracted texttext/plain260350http://repositorio.ufsm.br/bitstream/1/4219/2/FRIGGI%2c%20CAROLINE%20DO%20AMARAL.pdf.txtc22043db130302e51069ad6532ece4d2MD52THUMBNAILFRIGGI, CAROLINE DO AMARAL.pdf.jpgFRIGGI, CAROLINE DO AMARAL.pdf.jpgIM Thumbnailimage/jpeg6013http://repositorio.ufsm.br/bitstream/1/4219/3/FRIGGI%2c%20CAROLINE%20DO%20AMARAL.pdf.jpga7ccd9e675b7954329bc05300c3b6d62MD531/42192022-05-18 10:59:29.657oai:repositorio.ufsm.br:1/4219Biblioteca Digital de Teses e Dissertaçõeshttps://repositorio.ufsm.br/ONGhttps://repositorio.ufsm.br/oai/requestatendimento.sib@ufsm.br||tedebc@gmail.comopendoar:2022-05-18T13:59:29Biblioteca Digital de Teses e Dissertações do UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Determinação multiclasse de resíduos de agrotóxicos e medicamentos veterinários em carnes por LC-MS/MS |
dc.title.alternative.eng.fl_str_mv |
Multiclass determination of pesticides and veterinary drugs residues in meat by LC-MS/MS |
title |
Determinação multiclasse de resíduos de agrotóxicos e medicamentos veterinários em carnes por LC-MS/MS |
spellingShingle |
Determinação multiclasse de resíduos de agrotóxicos e medicamentos veterinários em carnes por LC-MS/MS Friggi, Caroline do Amaral Carnes Agrotóxicos Medicamentos veterinários QuEChERS LCMS/MS Meat Pesticides Veterinary drugs CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Determinação multiclasse de resíduos de agrotóxicos e medicamentos veterinários em carnes por LC-MS/MS |
title_full |
Determinação multiclasse de resíduos de agrotóxicos e medicamentos veterinários em carnes por LC-MS/MS |
title_fullStr |
Determinação multiclasse de resíduos de agrotóxicos e medicamentos veterinários em carnes por LC-MS/MS |
title_full_unstemmed |
Determinação multiclasse de resíduos de agrotóxicos e medicamentos veterinários em carnes por LC-MS/MS |
title_sort |
Determinação multiclasse de resíduos de agrotóxicos e medicamentos veterinários em carnes por LC-MS/MS |
author |
Friggi, Caroline do Amaral |
author_facet |
Friggi, Caroline do Amaral |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Zanella, Renato |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/2541865299438479 |
dc.contributor.advisor-co1.fl_str_mv |
Adaime, Martha Bohrer |
dc.contributor.advisor-co1Lattes.fl_str_mv |
http://lattes.cnpq.br/4385786922516848 |
dc.contributor.referee1.fl_str_mv |
Rath, Susanne |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/4317826174161775 |
dc.contributor.referee2.fl_str_mv |
Prestes, Osmar Damian |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/9632234955509028 |
dc.contributor.referee3.fl_str_mv |
Richards, Neila Silvia Pereira dos Santos |
dc.contributor.referee3Lattes.fl_str_mv |
http://lattes.cnpq.br/0618653776990780 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/8099993750354618 |
dc.contributor.author.fl_str_mv |
Friggi, Caroline do Amaral |
contributor_str_mv |
Zanella, Renato Adaime, Martha Bohrer Rath, Susanne Prestes, Osmar Damian Richards, Neila Silvia Pereira dos Santos |
dc.subject.por.fl_str_mv |
Carnes Agrotóxicos Medicamentos veterinários QuEChERS LCMS/MS |
topic |
Carnes Agrotóxicos Medicamentos veterinários QuEChERS LCMS/MS Meat Pesticides Veterinary drugs CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Meat Pesticides Veterinary drugs |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
The agribusiness has been incorporating new technologies in the production of meat, including good management of farms, health, balanced diet, breeding and integrated production. Allied to this, there is a growing concern with issues related to residues and contaminants in animals intended for food production. In the study, were compared four extraction methods based on the method QuEChERS for the determination of 79 pesticides and 15 veterinary drugs analyzed by Liquid Chromatography coupled to tandem Mass Spectrometry in samples of meat and pork liver, chicken and fish. The parameters evaluated were: linear range (6 concentration levels and 6 injections each), limit of detection (LOD), limit of quantification (LOQ), decision limit (CCα), capability of detection (CCβ) and matrix effect, as well as precision and accuracy, in terms of recovery. For this, we performed the fortification of matrices previously homogenized with solutions containing compounds at 3 levels of fortification (20, 50 and 100 μg kg-1), 6 replicates for each level, were performade. The modified QuEChERS extraction method consists in the extraction of 10 g of the matrix with 10 mL of acetonitrile containing 1% (v/v) of acetic acid and shaking vigorously by hand for 1 min. After, 4 g of anhydrous magnesium sulfate and 1.7 g anhydrous sodium acetate were added and the agitation repeated. After the extract was centrifugated for 8 min (3500 rpm) and 2 mL of the extract was transferred to another tube containing 300 mg of anhydrous magnesium sulfate and 50 mg of sorbent PSA, repeating the agitation and centrifugation. The extract was diluted (1:1 v/v) in the mobile phase and then analyzed by LC-MS/MS. Analytical curves prepared in solvent and in extracts of matrices evaluated showed adequate linearity between 5 and 200 μg kg-1, with coefficients of determination greater than 0.99. The method showed satisfactory recovery values between 70 and 120% (RSD ≤ 20%) to about 95% of compounds in all matrices, except for liver showed satisfactory values to about 80% of the compound at levels of 20, 50 and 100 μg kg-1. The LOQ of method was 10 μg kg-1. CCα values were between 1.1 and 102.9 μg kg-1 and CCβ values were in the range 1.9 to 105.9 μg kg-1. The results of this study showed that the modified method QuEChERS is fast, simple and efficient and can be applied to the determination of pesticides and veterinary drugs in samples of meat and liver pork, chicken and fish fillet for routine analysis. Furthermore, the use of LC-MS/MS was efficent, allowing the determination and confirmation of a large number of compounds simultaneously at residues livels. |
publishDate |
2012 |
dc.date.issued.fl_str_mv |
2012-03-23 |
dc.date.accessioned.fl_str_mv |
2017-05-11 |
dc.date.available.fl_str_mv |
2017-05-11 |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/doctoralThesis |
format |
doctoralThesis |
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publishedVersion |
dc.identifier.citation.fl_str_mv |
FRIGGI, Caroline do Amaral. Multiclass determination of pesticides and veterinary drugs residues in meat by LC-MS/MS. 2012. 151 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2012. |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/4219 |
identifier_str_mv |
FRIGGI, Caroline do Amaral. Multiclass determination of pesticides and veterinary drugs residues in meat by LC-MS/MS. 2012. 151 f. Tese (Doutorado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2012. |
url |
http://repositorio.ufsm.br/handle/1/4219 |
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por |
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100600000000 |
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Universidade Federal de Santa Maria |
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Programa de Pós-Graduação em Química |
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UFSM |
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Química |
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Universidade Federal de Santa Maria |
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