The application of quality by design in the development of the liquid chromatography method to determine empagliflozin in the presence of its organic impurities
Autor(a) principal: | |
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Data de Publicação: | 2020 |
Outros Autores: | , , , , , , |
Tipo de documento: | Artigo |
Idioma: | eng |
Título da fonte: | Repositório Institucional da UFRGS |
Texto Completo: | http://hdl.handle.net/10183/210732 |
Resumo: | Analysis of impurities is an important step in the quality control of pharmaceutical ingredients and final products. From drug synthesis or excipients, even in small concentrations, impurities may affect efficacy and safety. The method was developed following Quality by Design (QbD) for the analysis of the antidiabetic empagliflozin. The concept of QbD is used as a tool for the development of methods and formulations. Through predefined objectives and risk analysis, robust methodologies and reduced solvent consumption are developed. A simple HPLC method was developed and validated for the quantitative determination of empagliflozin and its organic impurities from the synthesis process. The method was carried out in a Shim-pack phenyl column with a mobile phase consisting of an acetonitrile/ water mixture (72 : 28), with isocratic elution and the detector wavelength was 230 nm. The validation process, in accordance with international guidelines, shows that the method was linear, precise and accurate for empagliflozin, impurity 1 and impurity 2. Limits of detection (0.01, 0.02 and 0.01 mg mL 1) and quantification (0.10, 0.10 and 0.05 mg mL 1) were determined for EMPA, IMP1 and IMP2, respectively. The HPLC method for impurity determination in empagliflozin was linear, precise, accurate and robust. It can be successfully applied in the quality control of empagliflozin and the synthesis of impurities, being adequate for routine analysis. |
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Manoel, Joanna WittckindPrimieri, Gabriele BordignonBueno, Lívia MaronesiWingert, Nathalie RibeiroVolpato, Nadia MariaGarcia, Cassia VirginiaSchapoval, Elfrides Eva SchermanSteppe, Martin2020-06-27T03:39:53Z20202046-2069http://hdl.handle.net/10183/210732001114260Analysis of impurities is an important step in the quality control of pharmaceutical ingredients and final products. From drug synthesis or excipients, even in small concentrations, impurities may affect efficacy and safety. The method was developed following Quality by Design (QbD) for the analysis of the antidiabetic empagliflozin. The concept of QbD is used as a tool for the development of methods and formulations. Through predefined objectives and risk analysis, robust methodologies and reduced solvent consumption are developed. A simple HPLC method was developed and validated for the quantitative determination of empagliflozin and its organic impurities from the synthesis process. The method was carried out in a Shim-pack phenyl column with a mobile phase consisting of an acetonitrile/ water mixture (72 : 28), with isocratic elution and the detector wavelength was 230 nm. The validation process, in accordance with international guidelines, shows that the method was linear, precise and accurate for empagliflozin, impurity 1 and impurity 2. Limits of detection (0.01, 0.02 and 0.01 mg mL 1) and quantification (0.10, 0.10 and 0.05 mg mL 1) were determined for EMPA, IMP1 and IMP2, respectively. The HPLC method for impurity determination in empagliflozin was linear, precise, accurate and robust. It can be successfully applied in the quality control of empagliflozin and the synthesis of impurities, being adequate for routine analysis.application/pdfengRSC Advances. Cambridge. Vol. 10 (2020), p. 7313-7320FarmáciaCromatografia líquidaContaminação de medicamentosControle de qualidadeThe application of quality by design in the development of the liquid chromatography method to determine empagliflozin in the presence of its organic impuritiesEstrangeiroinfo:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFRGSinstname:Universidade Federal do Rio Grande do Sul (UFRGS)instacron:UFRGSTEXT001114260.pdf.txt001114260.pdf.txtExtracted Texttext/plain37138http://www.lume.ufrgs.br/bitstream/10183/210732/2/001114260.pdf.txt1fddf8af3f0a6d6158a191e655f56d5fMD52ORIGINAL001114260.pdfTexto completo (inglês)application/pdf458548http://www.lume.ufrgs.br/bitstream/10183/210732/1/001114260.pdf5f14339af0080dc890e4a31e0d2ca72bMD5110183/2107322020-06-28 03:34:13.713603oai:www.lume.ufrgs.br:10183/210732Repositório de PublicaçõesPUBhttps://lume.ufrgs.br/oai/requestopendoar:2020-06-28T06:34:13Repositório Institucional da UFRGS - Universidade Federal do Rio Grande do Sul (UFRGS)false |
dc.title.pt_BR.fl_str_mv |
The application of quality by design in the development of the liquid chromatography method to determine empagliflozin in the presence of its organic impurities |
title |
The application of quality by design in the development of the liquid chromatography method to determine empagliflozin in the presence of its organic impurities |
spellingShingle |
The application of quality by design in the development of the liquid chromatography method to determine empagliflozin in the presence of its organic impurities Manoel, Joanna Wittckind Farmácia Cromatografia líquida Contaminação de medicamentos Controle de qualidade |
title_short |
The application of quality by design in the development of the liquid chromatography method to determine empagliflozin in the presence of its organic impurities |
title_full |
The application of quality by design in the development of the liquid chromatography method to determine empagliflozin in the presence of its organic impurities |
title_fullStr |
The application of quality by design in the development of the liquid chromatography method to determine empagliflozin in the presence of its organic impurities |
title_full_unstemmed |
The application of quality by design in the development of the liquid chromatography method to determine empagliflozin in the presence of its organic impurities |
title_sort |
The application of quality by design in the development of the liquid chromatography method to determine empagliflozin in the presence of its organic impurities |
author |
Manoel, Joanna Wittckind |
author_facet |
Manoel, Joanna Wittckind Primieri, Gabriele Bordignon Bueno, Lívia Maronesi Wingert, Nathalie Ribeiro Volpato, Nadia Maria Garcia, Cassia Virginia Schapoval, Elfrides Eva Scherman Steppe, Martin |
author_role |
author |
author2 |
Primieri, Gabriele Bordignon Bueno, Lívia Maronesi Wingert, Nathalie Ribeiro Volpato, Nadia Maria Garcia, Cassia Virginia Schapoval, Elfrides Eva Scherman Steppe, Martin |
author2_role |
author author author author author author author |
dc.contributor.author.fl_str_mv |
Manoel, Joanna Wittckind Primieri, Gabriele Bordignon Bueno, Lívia Maronesi Wingert, Nathalie Ribeiro Volpato, Nadia Maria Garcia, Cassia Virginia Schapoval, Elfrides Eva Scherman Steppe, Martin |
dc.subject.por.fl_str_mv |
Farmácia Cromatografia líquida Contaminação de medicamentos Controle de qualidade |
topic |
Farmácia Cromatografia líquida Contaminação de medicamentos Controle de qualidade |
description |
Analysis of impurities is an important step in the quality control of pharmaceutical ingredients and final products. From drug synthesis or excipients, even in small concentrations, impurities may affect efficacy and safety. The method was developed following Quality by Design (QbD) for the analysis of the antidiabetic empagliflozin. The concept of QbD is used as a tool for the development of methods and formulations. Through predefined objectives and risk analysis, robust methodologies and reduced solvent consumption are developed. A simple HPLC method was developed and validated for the quantitative determination of empagliflozin and its organic impurities from the synthesis process. The method was carried out in a Shim-pack phenyl column with a mobile phase consisting of an acetonitrile/ water mixture (72 : 28), with isocratic elution and the detector wavelength was 230 nm. The validation process, in accordance with international guidelines, shows that the method was linear, precise and accurate for empagliflozin, impurity 1 and impurity 2. Limits of detection (0.01, 0.02 and 0.01 mg mL 1) and quantification (0.10, 0.10 and 0.05 mg mL 1) were determined for EMPA, IMP1 and IMP2, respectively. The HPLC method for impurity determination in empagliflozin was linear, precise, accurate and robust. It can be successfully applied in the quality control of empagliflozin and the synthesis of impurities, being adequate for routine analysis. |
publishDate |
2020 |
dc.date.accessioned.fl_str_mv |
2020-06-27T03:39:53Z |
dc.date.issued.fl_str_mv |
2020 |
dc.type.driver.fl_str_mv |
Estrangeiro info:eu-repo/semantics/article |
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http://hdl.handle.net/10183/210732 |
dc.identifier.issn.pt_BR.fl_str_mv |
2046-2069 |
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001114260 |
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2046-2069 001114260 |
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http://hdl.handle.net/10183/210732 |
dc.language.iso.fl_str_mv |
eng |
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dc.relation.ispartof.pt_BR.fl_str_mv |
RSC Advances. Cambridge. Vol. 10 (2020), p. 7313-7320 |
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openAccess |
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