Desenvolvimento de métodos de preparo de amostras para a determinação de impurezas elementares em medicamentos de uso oral
Ano de defesa: | 2019 |
---|---|
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
Centro de Ciências Naturais e Exatas |
Programa de Pós-Graduação: |
Programa de Pós-Graduação em Química
|
Departamento: |
Química
|
País: |
Brasil
|
Palavras-chave em Português: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | http://repositorio.ufsm.br/handle/1/20854 |
Resumo: | In this study, sample preparation methods were developed for the digestion of oral pharmaceutical drugs used in the treatment of type 2 diabetes, with the objective of quantifying elemental impurities from classes 1 (As, Cd, Hg and Pb) and 2A (Co, Ni and V) by inductively coupled plasma optical emission spectrometry (ICP-OES). For this, the microwave induced combustion (MIC), microwave-assisted wet digestion (MAWD) and microwave and ultraviolet-assisted wet digestion (MAWD-UV) methods were evaluated. Six pharmaceutical drugs from different classes, containing metformine hydrochloride (MET), glibenclamide (GLIB), pioglitazone hydrochloride (PIO), sitagliptin hydrochloride (SITA), canagliflozin (CANA) and repaglinide (REPA) were used for the development of the methods. The drugs MET and CANA were chosen for the optimization of the methods. For the MIC method, the reflux step (5 or 10 min), the absorbing solution (7 and 14.4 mol L-1 HNO3, mixtures of 14.4 mol L-1 HNO3, 12 mol L-1 HCl and H2O in the proportion of 1+1+1, and mixtures of 14.4 mol L-1 HNO3 and 12 mol L-1 HCl in the proportions of 1+1, 1+3 and 3+1), and the use of combustion aids (microcrystallin cellulose or NH4Cl) were evaluated. For the MAWD method, the irradiation time (45 or 55 min), the digestion solution (1, 2, 3, 7 or 14.4 mol L-1 HNO3), the addition of an auxiliary reagent (1 or 2 mL of 50% H2O2) and the use of simultaneous cooling during the digestion (60 m3 h-1 or 125 m3 h-1 air flow rate) were evaluated. As for the MAWD-UV method, the following conditions were used: 1 mol L-1 HNO3, irradiation program of 55 min with simultaneous cooling (air flow rate of 125 m3 h-1 ), with the auxiliary reagent being evaluated (1.6 or 3.2 mL of 50% H2O2). For all the procedures, both the carbon concentration and residual acidity were determined in the digests. The accuracy of the methods was evaluated based on analyte recovery after standard addition assays and, for the MAWD and MAWD-UV methods, by the digestion of certified reference materials (CRM). When using MIC, V recoveries were not possible for samples containing inorganic excipients. For the MAWD method, CANA digestion was possible using 3 mol L-1 HNO3, 1 mL of 50% H2O2 and a 55 min irradiation program. The digestion of the other samples was possible using 2 mol L-1 HNO3, 1 mL of 50% H2O2 and a 45 min irradiation program. By using MAWD-UV, it was possible to digest all samples using 1 mol L-1 HNO3, 1.6 mL of 50% H2O2 and a 55 min irradiation program. The resulting digests from the optimized methods contained low residual acidity and dissolved carbon, enabling the analytes’ determination free of interferences by ICP-OES. In this way, it was possible to develop efficient methods for the decomposition of oral pharmaceutical drugs and subsequent class 1 and 2A (ICH Q3D guidelines) elemental impurities determination. |
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2021-05-12T18:39:58Z2021-05-12T18:39:58Z2019-08-02http://repositorio.ufsm.br/handle/1/20854In this study, sample preparation methods were developed for the digestion of oral pharmaceutical drugs used in the treatment of type 2 diabetes, with the objective of quantifying elemental impurities from classes 1 (As, Cd, Hg and Pb) and 2A (Co, Ni and V) by inductively coupled plasma optical emission spectrometry (ICP-OES). For this, the microwave induced combustion (MIC), microwave-assisted wet digestion (MAWD) and microwave and ultraviolet-assisted wet digestion (MAWD-UV) methods were evaluated. Six pharmaceutical drugs from different classes, containing metformine hydrochloride (MET), glibenclamide (GLIB), pioglitazone hydrochloride (PIO), sitagliptin hydrochloride (SITA), canagliflozin (CANA) and repaglinide (REPA) were used for the development of the methods. The drugs MET and CANA were chosen for the optimization of the methods. For the MIC method, the reflux step (5 or 10 min), the absorbing solution (7 and 14.4 mol L-1 HNO3, mixtures of 14.4 mol L-1 HNO3, 12 mol L-1 HCl and H2O in the proportion of 1+1+1, and mixtures of 14.4 mol L-1 HNO3 and 12 mol L-1 HCl in the proportions of 1+1, 1+3 and 3+1), and the use of combustion aids (microcrystallin cellulose or NH4Cl) were evaluated. For the MAWD method, the irradiation time (45 or 55 min), the digestion solution (1, 2, 3, 7 or 14.4 mol L-1 HNO3), the addition of an auxiliary reagent (1 or 2 mL of 50% H2O2) and the use of simultaneous cooling during the digestion (60 m3 h-1 or 125 m3 h-1 air flow rate) were evaluated. As for the MAWD-UV method, the following conditions were used: 1 mol L-1 HNO3, irradiation program of 55 min with simultaneous cooling (air flow rate of 125 m3 h-1 ), with the auxiliary reagent being evaluated (1.6 or 3.2 mL of 50% H2O2). For all the procedures, both the carbon concentration and residual acidity were determined in the digests. The accuracy of the methods was evaluated based on analyte recovery after standard addition assays and, for the MAWD and MAWD-UV methods, by the digestion of certified reference materials (CRM). When using MIC, V recoveries were not possible for samples containing inorganic excipients. For the MAWD method, CANA digestion was possible using 3 mol L-1 HNO3, 1 mL of 50% H2O2 and a 55 min irradiation program. The digestion of the other samples was possible using 2 mol L-1 HNO3, 1 mL of 50% H2O2 and a 45 min irradiation program. By using MAWD-UV, it was possible to digest all samples using 1 mol L-1 HNO3, 1.6 mL of 50% H2O2 and a 55 min irradiation program. The resulting digests from the optimized methods contained low residual acidity and dissolved carbon, enabling the analytes’ determination free of interferences by ICP-OES. In this way, it was possible to develop efficient methods for the decomposition of oral pharmaceutical drugs and subsequent class 1 and 2A (ICH Q3D guidelines) elemental impurities determination.Neste trabalho, foram desenvolvidos métodos de decomposição de medicamentos de uso oral utilizados no tratamento da diabetes tipo 2, na sua forma comercial, visando à determinação de impurezas elementares das classes 1 (As, Cd, Hg e Pb) e 2A (Co, Ni e V) por espectrometria de emissão óptica com plasma indutivamente acoplado (ICP-OES). Foram avaliados os métodos de combustão iniciada por micro-ondas (MIC), decomposição por via úmida assistida por radiação micro-ondas (MAWD) e decomposição por via úmida assistida por radiação micro- ondas e ultravioleta (MAWD-UV). Seis amostras de medicamentos de classes diferentes, à base de cloridrato de metformina (MET), glibenclamida (GLIB), cloridrato de pioglitazona (PIO), fosfato de sitagliptina (SITA), canagliflozina (CANA) e repaglinida (REPA) foram utilizados no desenvolvimento desse trabalho. Os medicamentos MET e CANA foram escolhidos para as otimizações dos métodos. Para a MIC, foram avaliados o tempo de refluxo (5 ou 10 min), a solução absorvedora (HNO3 7 e 14,4 mol L-1, misturas de HNO3 14,4 mol L-1, HCl 12 mol L-1 e H2O na proporção de 1+1+1, e misturas de HNO3 14,4 mol L-1 e HCl 12 mol L-1 nas proporções de 1+1, 1+3 e 3+1), e auxiliares de combustão (celulose microcristalina ou NH4Cl). Para a MAWD, foram avaliados o tempo de irradiação (45 ou 55 min), a solução digestora (HNO3 1, 2, 3, 7 ou 14,4 mol L-1), o reagente auxiliar (1 ou 2 mL de H2O2 50%), e o uso de resfriamento simultâneo (vazão de ar de 60 m3 h-1 ou 125 m3 h-1). No caso da MAWD-UV, foram utilizados HNO3 1 mol L-1, tempo de irradiação de 55 min com resfriamento simultâneo (vazão de ar de 125 m3 h-1), sendo avaliada a concentração do reagente auxiliar (1,6 ou 3,2 mL de H2O2 50%). Para todos os procedimentos, foi feita a determinação da concentração de carbono dissolvido e acidez residual nos digeridos. A exatidão foi avaliada com base em ensaios de recuperação com adição de padrão e, para os métodos de MAWD e MAWD-UV, pela decomposição de materiais de referência certificados (CRMs). Utilizando a MIC, não foi possível obter recuperações quantitativas para V em nenhuma das condições avaliadas em amostras com excipientes inorgânicos. Para a MAWD, a decomposição da CANA foi possível usando HNO3 3 mol L-1, 1 mL de H2O2 50% e programa de irradiação de 55 min. Para as demais amostras, a decomposição foi possível usando HNO3 2 mol L-1, 1 mL de H2O2 50% e tempo de irradiação de 45 min. Usando a MAWD-UV, foi possível decompor todas as amostras usando HNO3 1 mol L-1, 1,6 mL de H2O2 50% e programa de irradiação de 55 min. Os digeridos dos métodos de decomposição otimizados apresentaram baixo teor de acidez residual e carbono dissolvido, possibilitando a determinação por ICP-OES livre de interferências. Desta forma, foi possível desenvolver métodos eficientes para a decomposição da matriz orgânica de medicamentos de uso oral e posterior determinação de impurezas elementares das classes 1 e 2A do Guia ICH Q3D.Conselho Nacional de Pesquisa e Desenvolvimento Científico e Tecnológico - CNPqporUniversidade Federal de Santa MariaCentro de Ciências Naturais e ExatasPrograma de Pós-Graduação em QuímicaUFSMBrasilQuímicaAttribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/info:eu-repo/semantics/openAccessImpurezas elementaresMAWDMAWD-UVFármacosDiabetes tipo 2Elemental impuritiesPharmaceutical productsType 2 diabetesCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICADesenvolvimento de métodos de preparo de amostras para a determinação de impurezas elementares em medicamentos de uso oralDevelopment of sample preparation methods for elemental impurities determination in oral pharmaceutical drugsinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisFlores, Érico Marlon de Moraeshttp://lattes.cnpq.br/7167629055579212Costa, Adilson Ben daXXXXXXXXXXXXXXXMüller, Edson IrineuXXXXXXXXXXXXXXXXXXhttp://lattes.cnpq.br/9497575232006847Cauduro, Vitoria Hagemann100600000000600a9c2788c-7913-4d7b-92e1-3429800ac02815599056-5992-4735-8bf2-5c15abf572378fd7d402-38cb-487a-ae04-60b751dc48d66807df31-e8bb-413e-a246-d79076e2d085reponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALDIS_PPGQUIMICA_2019_CAUDURO_VITORIA.pdfDIS_PPGQUIMICA_2019_CAUDURO_VITORIA.pdfDissertação de Mestradoapplication/pdf1936380http://repositorio.ufsm.br/bitstream/1/20854/1/DIS_PPGQUIMICA_2019_CAUDURO_VITORIA.pdf5bd1a9387475ff67a41529ed7f677946MD51LICENSElicense.txtlicense.txttext/plain; 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dc.title.por.fl_str_mv |
Desenvolvimento de métodos de preparo de amostras para a determinação de impurezas elementares em medicamentos de uso oral |
dc.title.alternative.eng.fl_str_mv |
Development of sample preparation methods for elemental impurities determination in oral pharmaceutical drugs |
title |
Desenvolvimento de métodos de preparo de amostras para a determinação de impurezas elementares em medicamentos de uso oral |
spellingShingle |
Desenvolvimento de métodos de preparo de amostras para a determinação de impurezas elementares em medicamentos de uso oral Cauduro, Vitoria Hagemann Impurezas elementares MAWD MAWD-UV Fármacos Diabetes tipo 2 Elemental impurities Pharmaceutical products Type 2 diabetes CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Desenvolvimento de métodos de preparo de amostras para a determinação de impurezas elementares em medicamentos de uso oral |
title_full |
Desenvolvimento de métodos de preparo de amostras para a determinação de impurezas elementares em medicamentos de uso oral |
title_fullStr |
Desenvolvimento de métodos de preparo de amostras para a determinação de impurezas elementares em medicamentos de uso oral |
title_full_unstemmed |
Desenvolvimento de métodos de preparo de amostras para a determinação de impurezas elementares em medicamentos de uso oral |
title_sort |
Desenvolvimento de métodos de preparo de amostras para a determinação de impurezas elementares em medicamentos de uso oral |
author |
Cauduro, Vitoria Hagemann |
author_facet |
Cauduro, Vitoria Hagemann |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Flores, Érico Marlon de Moraes |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/7167629055579212 |
dc.contributor.referee1.fl_str_mv |
Costa, Adilson Ben da |
dc.contributor.referee1Lattes.fl_str_mv |
XXXXXXXXXXXXXXX |
dc.contributor.referee2.fl_str_mv |
Müller, Edson Irineu |
dc.contributor.referee2Lattes.fl_str_mv |
XXXXXXXXXXXXXXXXXX |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/9497575232006847 |
dc.contributor.author.fl_str_mv |
Cauduro, Vitoria Hagemann |
contributor_str_mv |
Flores, Érico Marlon de Moraes Costa, Adilson Ben da Müller, Edson Irineu |
dc.subject.por.fl_str_mv |
Impurezas elementares MAWD MAWD-UV Fármacos Diabetes tipo 2 |
topic |
Impurezas elementares MAWD MAWD-UV Fármacos Diabetes tipo 2 Elemental impurities Pharmaceutical products Type 2 diabetes CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Elemental impurities Pharmaceutical products Type 2 diabetes |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
In this study, sample preparation methods were developed for the digestion of oral pharmaceutical drugs used in the treatment of type 2 diabetes, with the objective of quantifying elemental impurities from classes 1 (As, Cd, Hg and Pb) and 2A (Co, Ni and V) by inductively coupled plasma optical emission spectrometry (ICP-OES). For this, the microwave induced combustion (MIC), microwave-assisted wet digestion (MAWD) and microwave and ultraviolet-assisted wet digestion (MAWD-UV) methods were evaluated. Six pharmaceutical drugs from different classes, containing metformine hydrochloride (MET), glibenclamide (GLIB), pioglitazone hydrochloride (PIO), sitagliptin hydrochloride (SITA), canagliflozin (CANA) and repaglinide (REPA) were used for the development of the methods. The drugs MET and CANA were chosen for the optimization of the methods. For the MIC method, the reflux step (5 or 10 min), the absorbing solution (7 and 14.4 mol L-1 HNO3, mixtures of 14.4 mol L-1 HNO3, 12 mol L-1 HCl and H2O in the proportion of 1+1+1, and mixtures of 14.4 mol L-1 HNO3 and 12 mol L-1 HCl in the proportions of 1+1, 1+3 and 3+1), and the use of combustion aids (microcrystallin cellulose or NH4Cl) were evaluated. For the MAWD method, the irradiation time (45 or 55 min), the digestion solution (1, 2, 3, 7 or 14.4 mol L-1 HNO3), the addition of an auxiliary reagent (1 or 2 mL of 50% H2O2) and the use of simultaneous cooling during the digestion (60 m3 h-1 or 125 m3 h-1 air flow rate) were evaluated. As for the MAWD-UV method, the following conditions were used: 1 mol L-1 HNO3, irradiation program of 55 min with simultaneous cooling (air flow rate of 125 m3 h-1 ), with the auxiliary reagent being evaluated (1.6 or 3.2 mL of 50% H2O2). For all the procedures, both the carbon concentration and residual acidity were determined in the digests. The accuracy of the methods was evaluated based on analyte recovery after standard addition assays and, for the MAWD and MAWD-UV methods, by the digestion of certified reference materials (CRM). When using MIC, V recoveries were not possible for samples containing inorganic excipients. For the MAWD method, CANA digestion was possible using 3 mol L-1 HNO3, 1 mL of 50% H2O2 and a 55 min irradiation program. The digestion of the other samples was possible using 2 mol L-1 HNO3, 1 mL of 50% H2O2 and a 45 min irradiation program. By using MAWD-UV, it was possible to digest all samples using 1 mol L-1 HNO3, 1.6 mL of 50% H2O2 and a 55 min irradiation program. The resulting digests from the optimized methods contained low residual acidity and dissolved carbon, enabling the analytes’ determination free of interferences by ICP-OES. In this way, it was possible to develop efficient methods for the decomposition of oral pharmaceutical drugs and subsequent class 1 and 2A (ICH Q3D guidelines) elemental impurities determination. |
publishDate |
2019 |
dc.date.issued.fl_str_mv |
2019-08-02 |
dc.date.accessioned.fl_str_mv |
2021-05-12T18:39:58Z |
dc.date.available.fl_str_mv |
2021-05-12T18:39:58Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/masterThesis |
format |
masterThesis |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/20854 |
url |
http://repositorio.ufsm.br/handle/1/20854 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 |
dc.relation.authority.fl_str_mv |
a9c2788c-7913-4d7b-92e1-3429800ac028 15599056-5992-4735-8bf2-5c15abf57237 8fd7d402-38cb-487a-ae04-60b751dc48d6 6807df31-e8bb-413e-a246-d79076e2d085 |
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.publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
dc.publisher.program.fl_str_mv |
Programa de Pós-Graduação em Química |
dc.publisher.initials.fl_str_mv |
UFSM |
dc.publisher.country.fl_str_mv |
Brasil |
dc.publisher.department.fl_str_mv |
Química |
publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
dc.source.none.fl_str_mv |
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Universidade Federal de Santa Maria (UFSM) |
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UFSM |
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UFSM |
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Manancial - Repositório Digital da UFSM |
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Manancial - Repositório Digital da UFSM |
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MD5 MD5 MD5 MD5 MD5 |
repository.name.fl_str_mv |
Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
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