Forced degradation of gliquidone and development of validated stability-indicating HPLC and TLC methods
Autor(a) principal: | |
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Data de Publicação: | 2018 |
Outros Autores: | , , |
Tipo de documento: | Artigo |
Idioma: | eng |
Título da fonte: | Brazilian Journal of Pharmaceutical Sciences |
Texto Completo: | https://www.revistas.usp.br/bjps/article/view/153830 |
Resumo: | Forced degradation studies of gliquidone were conducted under different stress conditions. Three degradates were observed upon using HPLC and TLC and elucidated by LC-MS and IR. HPLC method was performed on C18 column using methanol-water (85:15 v/v) pH 3.5 as a mobile phase with isocratic mode at 1 mL.min-1 and detection at 225 nm. HPLC analysis was applied in range of 0.5-20 µg.mL-1 (r =1) with limit of detection (LOD) 0.177 µg.mL-1. TLC method was based on the separation of gliquidone from degradation products on silica gel TLC F254 plates using chloroform-cyclohexaneglacial acetic acid (6:3:1v/v) as a developing system with relative retardation 1.15±0.01. Densitometric measurements were achieved in range of 2 -20 µg /band at 254 nm (r = 0.9999) with LOD of 0.26 µg /band. Least squares regression analysis was applied to provide mathematical estimates of the degree of linearity. The analysis revealed a linear calibration for HPLC where a binomial relationship for TLC. Stability testing and methods validation have been evaluated according to International Conference on Harmonization guidelines. Moreover, the proposed methods were applied for the analysis of tablets and the results obtained were statistically compared with those of pharmacopeial method revealing no significant difference about accuracy and precision. |
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Brazilian Journal of Pharmaceutical Sciences |
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Forced degradation of gliquidone and development of validated stability-indicating HPLC and TLC methodsGliquidone/forced degradation/stability-indicatingHPLC/method validationTLC/method validationForced degradation studies of gliquidone were conducted under different stress conditions. Three degradates were observed upon using HPLC and TLC and elucidated by LC-MS and IR. HPLC method was performed on C18 column using methanol-water (85:15 v/v) pH 3.5 as a mobile phase with isocratic mode at 1 mL.min-1 and detection at 225 nm. HPLC analysis was applied in range of 0.5-20 µg.mL-1 (r =1) with limit of detection (LOD) 0.177 µg.mL-1. TLC method was based on the separation of gliquidone from degradation products on silica gel TLC F254 plates using chloroform-cyclohexaneglacial acetic acid (6:3:1v/v) as a developing system with relative retardation 1.15±0.01. Densitometric measurements were achieved in range of 2 -20 µg /band at 254 nm (r = 0.9999) with LOD of 0.26 µg /band. Least squares regression analysis was applied to provide mathematical estimates of the degree of linearity. The analysis revealed a linear calibration for HPLC where a binomial relationship for TLC. Stability testing and methods validation have been evaluated according to International Conference on Harmonization guidelines. Moreover, the proposed methods were applied for the analysis of tablets and the results obtained were statistically compared with those of pharmacopeial method revealing no significant difference about accuracy and precision.Universidade de São Paulo. Faculdade de Ciências Farmacêuticas2018-11-29info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionapplication/pdfhttps://www.revistas.usp.br/bjps/article/view/15383010.1590/s2175-97902018000317223Brazilian Journal of Pharmaceutical Sciences; Vol. 54 Núm. 3 (2018); e00223Brazilian Journal of Pharmaceutical Sciences; v. 54 n. 3 (2018); e00223Brazilian Journal of Pharmaceutical Sciences; Vol. 54 No. 3 (2018); e002232175-97901984-8250reponame:Brazilian Journal of Pharmaceutical Sciencesinstname:Universidade de São Paulo (USP)instacron:USPenghttps://www.revistas.usp.br/bjps/article/view/153830/150197Copyright (c) 2018 Brazilian Journal of Pharmaceutical Sciences (Impresso)info:eu-repo/semantics/openAccessEl-ghobashy, Mohamed RefaatYehia, Ali MohamedHelmy, Aya HelmyYoussef, Nadia Fayek2019-03-17T12:48:22Zoai:revistas.usp.br:article/153830Revistahttps://www.revistas.usp.br/bjps/indexPUBhttps://old.scielo.br/oai/scielo-oai.phpbjps@usp.br||elizabeth.igne@gmail.com2175-97901984-8250opendoar:2019-03-17T12:48:22Brazilian Journal of Pharmaceutical Sciences - Universidade de São Paulo (USP)false |
dc.title.none.fl_str_mv |
Forced degradation of gliquidone and development of validated stability-indicating HPLC and TLC methods |
title |
Forced degradation of gliquidone and development of validated stability-indicating HPLC and TLC methods |
spellingShingle |
Forced degradation of gliquidone and development of validated stability-indicating HPLC and TLC methods El-ghobashy, Mohamed Refaat Gliquidone/forced degradation/stability-indicating HPLC/method validation TLC/method validation |
title_short |
Forced degradation of gliquidone and development of validated stability-indicating HPLC and TLC methods |
title_full |
Forced degradation of gliquidone and development of validated stability-indicating HPLC and TLC methods |
title_fullStr |
Forced degradation of gliquidone and development of validated stability-indicating HPLC and TLC methods |
title_full_unstemmed |
Forced degradation of gliquidone and development of validated stability-indicating HPLC and TLC methods |
title_sort |
Forced degradation of gliquidone and development of validated stability-indicating HPLC and TLC methods |
author |
El-ghobashy, Mohamed Refaat |
author_facet |
El-ghobashy, Mohamed Refaat Yehia, Ali Mohamed Helmy, Aya Helmy Youssef, Nadia Fayek |
author_role |
author |
author2 |
Yehia, Ali Mohamed Helmy, Aya Helmy Youssef, Nadia Fayek |
author2_role |
author author author |
dc.contributor.author.fl_str_mv |
El-ghobashy, Mohamed Refaat Yehia, Ali Mohamed Helmy, Aya Helmy Youssef, Nadia Fayek |
dc.subject.por.fl_str_mv |
Gliquidone/forced degradation/stability-indicating HPLC/method validation TLC/method validation |
topic |
Gliquidone/forced degradation/stability-indicating HPLC/method validation TLC/method validation |
description |
Forced degradation studies of gliquidone were conducted under different stress conditions. Three degradates were observed upon using HPLC and TLC and elucidated by LC-MS and IR. HPLC method was performed on C18 column using methanol-water (85:15 v/v) pH 3.5 as a mobile phase with isocratic mode at 1 mL.min-1 and detection at 225 nm. HPLC analysis was applied in range of 0.5-20 µg.mL-1 (r =1) with limit of detection (LOD) 0.177 µg.mL-1. TLC method was based on the separation of gliquidone from degradation products on silica gel TLC F254 plates using chloroform-cyclohexaneglacial acetic acid (6:3:1v/v) as a developing system with relative retardation 1.15±0.01. Densitometric measurements were achieved in range of 2 -20 µg /band at 254 nm (r = 0.9999) with LOD of 0.26 µg /band. Least squares regression analysis was applied to provide mathematical estimates of the degree of linearity. The analysis revealed a linear calibration for HPLC where a binomial relationship for TLC. Stability testing and methods validation have been evaluated according to International Conference on Harmonization guidelines. Moreover, the proposed methods were applied for the analysis of tablets and the results obtained were statistically compared with those of pharmacopeial method revealing no significant difference about accuracy and precision. |
publishDate |
2018 |
dc.date.none.fl_str_mv |
2018-11-29 |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/article info:eu-repo/semantics/publishedVersion |
format |
article |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
https://www.revistas.usp.br/bjps/article/view/153830 10.1590/s2175-97902018000317223 |
url |
https://www.revistas.usp.br/bjps/article/view/153830 |
identifier_str_mv |
10.1590/s2175-97902018000317223 |
dc.language.iso.fl_str_mv |
eng |
language |
eng |
dc.relation.none.fl_str_mv |
https://www.revistas.usp.br/bjps/article/view/153830/150197 |
dc.rights.driver.fl_str_mv |
Copyright (c) 2018 Brazilian Journal of Pharmaceutical Sciences (Impresso) info:eu-repo/semantics/openAccess |
rights_invalid_str_mv |
Copyright (c) 2018 Brazilian Journal of Pharmaceutical Sciences (Impresso) |
eu_rights_str_mv |
openAccess |
dc.format.none.fl_str_mv |
application/pdf |
dc.publisher.none.fl_str_mv |
Universidade de São Paulo. Faculdade de Ciências Farmacêuticas |
publisher.none.fl_str_mv |
Universidade de São Paulo. Faculdade de Ciências Farmacêuticas |
dc.source.none.fl_str_mv |
Brazilian Journal of Pharmaceutical Sciences; Vol. 54 Núm. 3 (2018); e00223 Brazilian Journal of Pharmaceutical Sciences; v. 54 n. 3 (2018); e00223 Brazilian Journal of Pharmaceutical Sciences; Vol. 54 No. 3 (2018); e00223 2175-9790 1984-8250 reponame:Brazilian Journal of Pharmaceutical Sciences instname:Universidade de São Paulo (USP) instacron:USP |
instname_str |
Universidade de São Paulo (USP) |
instacron_str |
USP |
institution |
USP |
reponame_str |
Brazilian Journal of Pharmaceutical Sciences |
collection |
Brazilian Journal of Pharmaceutical Sciences |
repository.name.fl_str_mv |
Brazilian Journal of Pharmaceutical Sciences - Universidade de São Paulo (USP) |
repository.mail.fl_str_mv |
bjps@usp.br||elizabeth.igne@gmail.com |
_version_ |
1800222913761116160 |