Validation of a HPLC-UV analytical and bioanalytical method for dexamethasone determination in nanoemulsions, porcine nasal mucosa, and mouse plasma and brain tissue

Dexamethasone (DEX) is a synthetic glucocorticoid widely used in the treatment of inflammatory and autoimmune diseases. However, its clinical efficacy is limited by low water solubility, poor bioavailability, and a high incidence of side effects. To overcome these limitations, nanotechnology-based...

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Main Authors: Luísa Degrandi Sehn, Gabriela Fusinatto de Oliveira, Melaine Maiara da Silva Lopes, Helder Ferreira Teixeira, Ursula da Silveira Matte, Roselena Silvestri Schuh, Flavia Fachel
Format: Article
Language:English
Published: Universidade Federal do Rio Grande do Sul 2025-07-01
Series:Drug Analytical Research
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Online Access:https://seer.ufrgs.br/index.php/dar/article/view/148019
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author Luísa Degrandi Sehn
Gabriela Fusinatto de Oliveira
Melaine Maiara da Silva Lopes
Helder Ferreira Teixeira
Ursula da Silveira Matte
Roselena Silvestri Schuh
Flavia Fachel
author_facet Luísa Degrandi Sehn
Gabriela Fusinatto de Oliveira
Melaine Maiara da Silva Lopes
Helder Ferreira Teixeira
Ursula da Silveira Matte
Roselena Silvestri Schuh
Flavia Fachel
author_sort Luísa Degrandi Sehn
collection DOAJ
description Dexamethasone (DEX) is a synthetic glucocorticoid widely used in the treatment of inflammatory and autoimmune diseases. However, its clinical efficacy is limited by low water solubility, poor bioavailability, and a high incidence of side effects. To overcome these limitations, nanotechnology-based drug delivery systems, such as nanoemulsions, have emerged as promising alternatives, particularly when combined with nasal administration targeting the treatment of neuroinflammation in the central nervous system. This study describes the validation of an analytical and bioanalytical method using high-performance liquid chromatography with ultraviolet detection (HPLC-UV) for the quantification of DEX active pharmaceutical ingredient (API) in nanoemulsions, porcine nasal mucosa, and mouse plasma and brain tissue. The method was validated according to current regulatory guidelines and was based on a procedure previously described in the 7th edition of the Brazilian Pharmacopoeia (2024). The method demonstrated specificity, with no interference from endogenous components of the matrices. Linearity was confirmed in the range of 0.5 to 10.0 µg mL⁻¹ for standard solutions, nanoemulsion, porcine nasal mucosa, and mouse plasma, and from 1.0 to 10.0 µg mL⁻¹ for mouse brain samples, with correlation coefficients (r) greater than 0.99. The method has also been shown to be precise, accurate and with low matrix effect within regulatory acceptance criteria. These results confirm the method’s reliability for determination of DEX in both nanotechnological and biological matrices. The validated method is intended to support future performance studies of nanotechnology-based formulations for nasal administration of DEX.
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spelling doaj-art-c3de5a498b7b49e1b11ceac38af26b492025-08-20T02:39:37ZengUniversidade Federal do Rio Grande do SulDrug Analytical Research2527-26162025-07-019110.22456/2527-2616.148019Validation of a HPLC-UV analytical and bioanalytical method for dexamethasone determination in nanoemulsions, porcine nasal mucosa, and mouse plasma and brain tissueLuísa Degrandi Sehn0https://orcid.org/0009-0001-6044-7512Gabriela Fusinatto de Oliveira1https://orcid.org/0009-0002-1628-8574Melaine Maiara da Silva Lopes2https://orcid.org/0000-0002-8474-137XHelder Ferreira Teixeira3https://orcid.org/0000-0002-5808-3043Ursula da Silveira Matte 4https://orcid.org/0000-0003-4977-6662Roselena Silvestri Schuh 5https://orcid.org/0000-0003-4189-0436Flavia Fachel6https://orcid.org/0000-0002-0777-9497Programa de Pós‐Graduação em Ciências Farmacêuticas, Faculdade de Farmácia, Universidade Federal do Rio Grande do Sul (UFRGS)Programa de Pós‐Graduação em Ciências Farmacêuticas, Faculdade de Farmácia, Universidade Federal do Rio Grande do Sul (UFRGS)Programa de Pós‐Graduação em Ciências Farmacêuticas, Faculdade de Farmácia, Universidade Federal do Rio Grande do Sul (UFRGS)Programa de Pós‐Graduação em Ciências Farmacêuticas, Faculdade de Farmácia, Universidade Federal do Rio Grande do Sul (UFRGS)Células, Tecidos e Genes, Centro de Pesquisa Experimental, Hospital de Clínicas de Porto AlegreCélulas, Tecidos e Genes, Centro de Pesquisa Experimental, Hospital de Clínicas de Porto Alegre, PPGCF- UFRGSPrograma de Pós‐Graduação em Ciências Farmacêuticas, Faculdade de Farmácia, Universidade Federal do Rio Grande do Sul (UFRGS) Dexamethasone (DEX) is a synthetic glucocorticoid widely used in the treatment of inflammatory and autoimmune diseases. However, its clinical efficacy is limited by low water solubility, poor bioavailability, and a high incidence of side effects. To overcome these limitations, nanotechnology-based drug delivery systems, such as nanoemulsions, have emerged as promising alternatives, particularly when combined with nasal administration targeting the treatment of neuroinflammation in the central nervous system. This study describes the validation of an analytical and bioanalytical method using high-performance liquid chromatography with ultraviolet detection (HPLC-UV) for the quantification of DEX active pharmaceutical ingredient (API) in nanoemulsions, porcine nasal mucosa, and mouse plasma and brain tissue. The method was validated according to current regulatory guidelines and was based on a procedure previously described in the 7th edition of the Brazilian Pharmacopoeia (2024). The method demonstrated specificity, with no interference from endogenous components of the matrices. Linearity was confirmed in the range of 0.5 to 10.0 µg mL⁻¹ for standard solutions, nanoemulsion, porcine nasal mucosa, and mouse plasma, and from 1.0 to 10.0 µg mL⁻¹ for mouse brain samples, with correlation coefficients (r) greater than 0.99. The method has also been shown to be precise, accurate and with low matrix effect within regulatory acceptance criteria. These results confirm the method’s reliability for determination of DEX in both nanotechnological and biological matrices. The validated method is intended to support future performance studies of nanotechnology-based formulations for nasal administration of DEX. https://seer.ufrgs.br/index.php/dar/article/view/148019DexamethasoneHPLCnanotechnologybiological matricesnasalplasma
spellingShingle Luísa Degrandi Sehn
Gabriela Fusinatto de Oliveira
Melaine Maiara da Silva Lopes
Helder Ferreira Teixeira
Ursula da Silveira Matte
Roselena Silvestri Schuh
Flavia Fachel
Validation of a HPLC-UV analytical and bioanalytical method for dexamethasone determination in nanoemulsions, porcine nasal mucosa, and mouse plasma and brain tissue
Drug Analytical Research
Dexamethasone
HPLC
nanotechnology
biological matrices
nasal
plasma
title Validation of a HPLC-UV analytical and bioanalytical method for dexamethasone determination in nanoemulsions, porcine nasal mucosa, and mouse plasma and brain tissue
title_full Validation of a HPLC-UV analytical and bioanalytical method for dexamethasone determination in nanoemulsions, porcine nasal mucosa, and mouse plasma and brain tissue
title_fullStr Validation of a HPLC-UV analytical and bioanalytical method for dexamethasone determination in nanoemulsions, porcine nasal mucosa, and mouse plasma and brain tissue
title_full_unstemmed Validation of a HPLC-UV analytical and bioanalytical method for dexamethasone determination in nanoemulsions, porcine nasal mucosa, and mouse plasma and brain tissue
title_short Validation of a HPLC-UV analytical and bioanalytical method for dexamethasone determination in nanoemulsions, porcine nasal mucosa, and mouse plasma and brain tissue
title_sort validation of a hplc uv analytical and bioanalytical method for dexamethasone determination in nanoemulsions porcine nasal mucosa and mouse plasma and brain tissue
topic Dexamethasone
HPLC
nanotechnology
biological matrices
nasal
plasma
url https://seer.ufrgs.br/index.php/dar/article/view/148019
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