Avaliação de um modulador a ar comprimido para GC×GC e sua aplicação para determinação de resíduos de pesticidas piretróides em uva
Ano de defesa: | 2008 |
---|---|
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: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/10424 |
Resumo: | In this study, a new modulator that is simple, robust and presents low operation costs was developed. This modulator uses compressed air to cool two small portions of the second chromatographic column of a GC×GC system. To evaluate the modulation process, solutions of alkanes C7 to C29, and pesticides (bifenthrin, cyfluthrin, cypermethrin, esfenvalerate, fenitrotion, fipronil, trifloxystrobin and trifluralin) were analyzed by GC×GC-FID. The results showed small variations of the peaks areas, between 0.67 and 2.80% for alkanes and between 0.24 and 5.34% for pesticides. The standard deviation (SD) for the retention time in the first column (1tR) was around 0.05 min, for alkanes and pesticides. For retention times in the second column (2tR), the SD was 0.04 s for the majority of the compounds, except for cyfluthrin and permethrin (0.08 s). The linear range was between 0.1 and 5.0 mg L-1 with a coefficient of determination (r2) greater than 0.9945 for pesticides analyzed by GC×GC-FID. The GC×GC system proposed was applied in the determination of pyrethroid pesticides (bifenthrin, cypermethrin, deltamethrin, fenvalerate and esfenvalerate and permethrin cis and trans) in grape samples Italy cultivar spiked at 3 levels (0.02, 0.05 and 0.5 mg kg- 1). Samples were extracted by the mini-Luke modified method (acetone method) and pesticides were quantified by GC×GC-μECD. The parameters evaluated in the validation of the method were: analytical curve, linearity, limit of detection (LOD), limit of quantification (LOQ), precision (in terms of repetitivity and intermediate precision) and accuracy (recovery), as well as the matrix effect on the chromatographic response. All analytical curves showed a linear range between 0.02 and 0.5 mg L-1 with r2 greater than 0.9956 and 0.9994 for the curves prepared in solvent (ethyl acetate) and matrix extract (grape), respectively. From the results obtained by calculation of the matrix effect percentage it can be concluded that the pyrethroid pesticides showed a considerable negative matrix effect. The values of method LOQ were 0.01 to 0.02 mg kg-1 for all pyrethroids. The values of recovery for the 3 spiked levels were between 94.3 and 115.2%, with good precision (RSD<18.4%), demonstrating that the performance of the mini-Luke modified method employed for the extractions is satisfactory. This study also showed that the GC×GC-μECD system using a modulator with a double jet of compressed air has potential for application in the analysis of pyrethroid pesticide residues in grapes, since it supplies low values of LOD and LOQ, and good accuracy in the analytical response. |
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2017-05-112017-05-112008-02-22FRIGGI, Caroline do Amaral. Evaluation of a compressed air modulator for GC×GC and application to determination of pyrethroid pesticides residues in grape. 2008. 107 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2008.http://repositorio.ufsm.br/handle/1/10424In this study, a new modulator that is simple, robust and presents low operation costs was developed. This modulator uses compressed air to cool two small portions of the second chromatographic column of a GC×GC system. To evaluate the modulation process, solutions of alkanes C7 to C29, and pesticides (bifenthrin, cyfluthrin, cypermethrin, esfenvalerate, fenitrotion, fipronil, trifloxystrobin and trifluralin) were analyzed by GC×GC-FID. The results showed small variations of the peaks areas, between 0.67 and 2.80% for alkanes and between 0.24 and 5.34% for pesticides. The standard deviation (SD) for the retention time in the first column (1tR) was around 0.05 min, for alkanes and pesticides. For retention times in the second column (2tR), the SD was 0.04 s for the majority of the compounds, except for cyfluthrin and permethrin (0.08 s). The linear range was between 0.1 and 5.0 mg L-1 with a coefficient of determination (r2) greater than 0.9945 for pesticides analyzed by GC×GC-FID. The GC×GC system proposed was applied in the determination of pyrethroid pesticides (bifenthrin, cypermethrin, deltamethrin, fenvalerate and esfenvalerate and permethrin cis and trans) in grape samples Italy cultivar spiked at 3 levels (0.02, 0.05 and 0.5 mg kg- 1). Samples were extracted by the mini-Luke modified method (acetone method) and pesticides were quantified by GC×GC-μECD. The parameters evaluated in the validation of the method were: analytical curve, linearity, limit of detection (LOD), limit of quantification (LOQ), precision (in terms of repetitivity and intermediate precision) and accuracy (recovery), as well as the matrix effect on the chromatographic response. All analytical curves showed a linear range between 0.02 and 0.5 mg L-1 with r2 greater than 0.9956 and 0.9994 for the curves prepared in solvent (ethyl acetate) and matrix extract (grape), respectively. From the results obtained by calculation of the matrix effect percentage it can be concluded that the pyrethroid pesticides showed a considerable negative matrix effect. The values of method LOQ were 0.01 to 0.02 mg kg-1 for all pyrethroids. The values of recovery for the 3 spiked levels were between 94.3 and 115.2%, with good precision (RSD<18.4%), demonstrating that the performance of the mini-Luke modified method employed for the extractions is satisfactory. This study also showed that the GC×GC-μECD system using a modulator with a double jet of compressed air has potential for application in the analysis of pyrethroid pesticide residues in grapes, since it supplies low values of LOD and LOQ, and good accuracy in the analytical response.Neste trabalho foi desenvolvido um novo modulador, simples, robusto e de baixo custo de operação. Este modulador utiliza ar comprimido para resfriar duas pequenas porções da segunda coluna cromatográfica de um sistema GC×GC. Para avaliar o processo de modulação utilizaram-se soluções de alcanos C7 a C29 e pesticidas (bifentrina, ciflutrina, cipermetrina, esfenvalerato, fenitrotiona, fipronil, trifloxistrobina e trifluralina) e análise por GC×GC-FID. Os resultados mostraram pequenas variações das áreas dos picos, entre 0,67 e 2,80% para alcanos e entre 0,24 e 5,34% para pesticidas. O desvio padrão (SD) para o tempo de retenção na primeira coluna (1tR) de alcanos e pesticidas foi em torno de 0,05 min. Para o tempo de retenção na segunda coluna (2tR), o SD foi de 0,04 s para a maioria dos compostos, exceto para ciflutrina e permetrina (0,08 s). A faixa linear situou-se entre 0,1 e 5,0 mg L-1 com coeficiente de determinação (r2) maior que 0,9945 para os pesticidas analisados por GC×GC-FID. O sistema GC×GC proposto foi aplicado na determinação de pesticidas piretróides (bifentrina, cipermetrina, deltametrina, fenvalerato e esfenvalerato, e permetrina cis e trans) em amostras de uva cultivar Itália fortificadas em 3 níveis (0,02; 0,05 e 0,5 mg kg-1). As amostras foram extraídas pelo método de mini-Luke modificado (método da acetona) e os pesticidas quantificados por GC×GC-μECD. Os parâmetros avaliados de validação do método foram: curva analítica, linearidade, limite de detecção (LOD), limite de quantificação (LOQ), precisão (em termos de repetitividade e precisão intermediária) e exatidão (recuperação), bem como o efeito matriz na resposta cromatográfica. Todas as curvas analíticas apresentaram faixa linear entre 0,02 e 0,5 mg L-1 com valores de r2 maiores que 0,9956 e 0,9994 para as curvas preparadas em solvente (acetato de etila) e extrato da matriz (uva), respectivamente. A partir dos resultados obtidos através do cálculo do efeito matriz percentual concluiu-se que os pesticidas piretróides avaliados apresentaram considerável efeito matriz negativo. Os valores de LOQ do método foram de 0,01 a 0,02 mg kg-1 para todos os piretróides. A recuperação para os 3 níveis de fortificação ficou entre 94,3 e 115,2%, com boa precisão (RSD<18,4%), o que mostrou que o desempenho do método mini-Luke modificado empregado para as extrações é satisfatório. Este estudo mostrou também, que o sistema GC×GC-μECD com modulador de duplo jato de ar comprimido tem potencial para aplicação nas análises de resíduos de pesticidas piretróides em uva, uma vez que fornece baixos valores de LOD e LOQ, e boa precisão da resposta analítica.Coordenação de Aperfeiçoamento de Pessoal de Nível Superiorapplication/pdfporUniversidade Federal de Santa MariaPrograma de Pós-Graduação em QuímicaUFSMBRQuímicaGC×GCModuladoresPesticidasFrutasModulatorsPesticidesFruitsCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICAAvaliação de um modulador a ar comprimido para GC×GC e sua aplicação para determinação de resíduos de pesticidas piretróides em uvaEvaluation of a compressed air modulator for GC×GC and application to determination of pyrethroid pesticides residues in grapeinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisZanella, Renatohttp://lattes.cnpq.br/2541865299438479Mühlen, Carin Vonhttp://lattes.cnpq.br/7555691352229740Adaime, Martha Bohrerhttp://lattes.cnpq.br/4385786922516848http://lattes.cnpq.br/8099993750354618Friggi, Caroline do Amaral1006000000004005005003005000aa2baab-94e8-4d3d-bbb2-85495ba77db5ee70933c-ddf1-4a31-bc29-ac954a4aa1ce58523d71-e405-44d3-a3a9-d4317a932eb0a0f5a1bf-e731-4df0-9010-ddadda7ae90ainfo:eu-repo/semantics/openAccessreponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALCAROLINEFRIGGI.pdfapplication/pdf3731017http://repositorio.ufsm.br/bitstream/1/10424/1/CAROLINEFRIGGI.pdfcf638b3d3720e9343456ebc2fb0eeaedMD51TEXTCAROLINEFRIGGI.pdf.txtCAROLINEFRIGGI.pdf.txtExtracted texttext/plain167492http://repositorio.ufsm.br/bitstream/1/10424/2/CAROLINEFRIGGI.pdf.txt8d7b47f9900be988f42c3c6530b44b20MD52THUMBNAILCAROLINEFRIGGI.pdf.jpgCAROLINEFRIGGI.pdf.jpgIM Thumbnailimage/jpeg6923http://repositorio.ufsm.br/bitstream/1/10424/3/CAROLINEFRIGGI.pdf.jpg4297a719eed2c5153d69b6afda7f44ecMD531/104242022-04-06 16:38:10.82oai:repositorio.ufsm.br:1/10424Repositório Institucionalhttp://repositorio.ufsm.br/PUBhttp://repositorio.ufsm.br/oai/requestopendoar:39132022-04-06T19:38:10Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM)false |
dc.title.por.fl_str_mv |
Avaliação de um modulador a ar comprimido para GC×GC e sua aplicação para determinação de resíduos de pesticidas piretróides em uva |
dc.title.alternative.eng.fl_str_mv |
Evaluation of a compressed air modulator for GC×GC and application to determination of pyrethroid pesticides residues in grape |
title |
Avaliação de um modulador a ar comprimido para GC×GC e sua aplicação para determinação de resíduos de pesticidas piretróides em uva |
spellingShingle |
Avaliação de um modulador a ar comprimido para GC×GC e sua aplicação para determinação de resíduos de pesticidas piretróides em uva Friggi, Caroline do Amaral GC×GC Moduladores Pesticidas Frutas Modulators Pesticides Fruits CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Avaliação de um modulador a ar comprimido para GC×GC e sua aplicação para determinação de resíduos de pesticidas piretróides em uva |
title_full |
Avaliação de um modulador a ar comprimido para GC×GC e sua aplicação para determinação de resíduos de pesticidas piretróides em uva |
title_fullStr |
Avaliação de um modulador a ar comprimido para GC×GC e sua aplicação para determinação de resíduos de pesticidas piretróides em uva |
title_full_unstemmed |
Avaliação de um modulador a ar comprimido para GC×GC e sua aplicação para determinação de resíduos de pesticidas piretróides em uva |
title_sort |
Avaliação de um modulador a ar comprimido para GC×GC e sua aplicação para determinação de resíduos de pesticidas piretróides em uva |
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.referee1.fl_str_mv |
Mühlen, Carin Von |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/7555691352229740 |
dc.contributor.referee2.fl_str_mv |
Adaime, Martha Bohrer |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/4385786922516848 |
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 Mühlen, Carin Von Adaime, Martha Bohrer |
dc.subject.por.fl_str_mv |
GC×GC Moduladores Pesticidas Frutas |
topic |
GC×GC Moduladores Pesticidas Frutas Modulators Pesticides Fruits CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Modulators Pesticides Fruits |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this study, a new modulator that is simple, robust and presents low operation costs was developed. This modulator uses compressed air to cool two small portions of the second chromatographic column of a GC×GC system. To evaluate the modulation process, solutions of alkanes C7 to C29, and pesticides (bifenthrin, cyfluthrin, cypermethrin, esfenvalerate, fenitrotion, fipronil, trifloxystrobin and trifluralin) were analyzed by GC×GC-FID. The results showed small variations of the peaks areas, between 0.67 and 2.80% for alkanes and between 0.24 and 5.34% for pesticides. The standard deviation (SD) for the retention time in the first column (1tR) was around 0.05 min, for alkanes and pesticides. For retention times in the second column (2tR), the SD was 0.04 s for the majority of the compounds, except for cyfluthrin and permethrin (0.08 s). The linear range was between 0.1 and 5.0 mg L-1 with a coefficient of determination (r2) greater than 0.9945 for pesticides analyzed by GC×GC-FID. The GC×GC system proposed was applied in the determination of pyrethroid pesticides (bifenthrin, cypermethrin, deltamethrin, fenvalerate and esfenvalerate and permethrin cis and trans) in grape samples Italy cultivar spiked at 3 levels (0.02, 0.05 and 0.5 mg kg- 1). Samples were extracted by the mini-Luke modified method (acetone method) and pesticides were quantified by GC×GC-μECD. The parameters evaluated in the validation of the method were: analytical curve, linearity, limit of detection (LOD), limit of quantification (LOQ), precision (in terms of repetitivity and intermediate precision) and accuracy (recovery), as well as the matrix effect on the chromatographic response. All analytical curves showed a linear range between 0.02 and 0.5 mg L-1 with r2 greater than 0.9956 and 0.9994 for the curves prepared in solvent (ethyl acetate) and matrix extract (grape), respectively. From the results obtained by calculation of the matrix effect percentage it can be concluded that the pyrethroid pesticides showed a considerable negative matrix effect. The values of method LOQ were 0.01 to 0.02 mg kg-1 for all pyrethroids. The values of recovery for the 3 spiked levels were between 94.3 and 115.2%, with good precision (RSD<18.4%), demonstrating that the performance of the mini-Luke modified method employed for the extractions is satisfactory. This study also showed that the GC×GC-μECD system using a modulator with a double jet of compressed air has potential for application in the analysis of pyrethroid pesticide residues in grapes, since it supplies low values of LOD and LOQ, and good accuracy in the analytical response. |
publishDate |
2008 |
dc.date.issued.fl_str_mv |
2008-02-22 |
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/masterThesis |
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masterThesis |
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publishedVersion |
dc.identifier.citation.fl_str_mv |
FRIGGI, Caroline do Amaral. Evaluation of a compressed air modulator for GC×GC and application to determination of pyrethroid pesticides residues in grape. 2008. 107 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2008. |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/10424 |
identifier_str_mv |
FRIGGI, Caroline do Amaral. Evaluation of a compressed air modulator for GC×GC and application to determination of pyrethroid pesticides residues in grape. 2008. 107 f. Dissertação (Mestrado em Química) - Universidade Federal de Santa Maria, Santa Maria, 2008. |
url |
http://repositorio.ufsm.br/handle/1/10424 |
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por |
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100600000000 |
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400 500 500 300 500 |
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info:eu-repo/semantics/openAccess |
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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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BR |
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Química |
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Universidade Federal de Santa Maria |
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