Determination of Methotrexate in pH-Sensitive Chitosan Nanoparticles by Validated RP-LC and UV Spectrophotometric Methods

Nanotechnology-based drug delivery systems are in constant development and, therefore, it is of great importance to have rapid, efficient and accurate analytical methodology to quantify the encapsulated drugs. Here, simple and fast methods, by reversed-phase liquid chromatography (RP-LC) and UV spec...

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Autores: Nogueira, Daniele R., Macedo, Letícia B., Scheeren, Laís E., Mitjans Arnal, Montserrat, Infante Martínez-Pardo, Ma. Rosa, Rolim, Clarice M. B., Vinardell Martínez-Hidalgo, Ma. Pilar
Tipo de recurso: artículo
Estado:Versión publicada
Fecha de publicación:2014
País:España
Institución:Varias* (Consorci de Biblioteques Universitáries de Catalunya, Centre de Serveis Científics i Acadèmics de Catalunya)
Repositorio:Recercat. Dipósit de la Recerca de Catalunya
OAI Identifier:oai:recercat.cat:2445/97209
Acceso en línea:https://hdl.handle.net/2445/97209
Access Level:acceso abierto
Palabra clave:Quitosan
Nanopartícules
Medicaments antineoplàstics
Metotrexat
Agents tensioactius
Cromatografia
Espectroscòpia
Chitosan
Nanoparticles
Antineoplastic agents
Methotrexate
Surface active agents
Chromatography
Spectrum analysis
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spelling Determination of Methotrexate in pH-Sensitive Chitosan Nanoparticles by Validated RP-LC and UV Spectrophotometric MethodsNogueira, Daniele R.Macedo, Letícia B.Scheeren, Laís E.Mitjans Arnal, MontserratInfante Martínez-Pardo, Ma. RosaRolim, Clarice M. B.Vinardell Martínez-Hidalgo, Ma. PilarQuitosanNanopartículesMedicaments antineoplàsticsMetotrexatAgents tensioactiusCromatografiaEspectroscòpiaChitosanNanoparticlesAntineoplastic agentsMethotrexateSurface active agentsChromatographySpectrum analysisNanotechnology-based drug delivery systems are in constant development and, therefore, it is of great importance to have rapid, efficient and accurate analytical methodology to quantify the encapsulated drugs. Here, simple and fast methods, by reversed-phase liquid chromatography (RP-LC) and UV spectrophotometry, were developed and validated for the determination of methotrexate (MTX) in pH-sensitive chitosan nanoparticles (CS-NPs). NPs were prepared using a modified ionotropic complexation process, in which was included a surfactant derived from Nα,Nε-dioctanoyl lysine with an inorganic sodium counterion. The RP-LC method was carried out on a Waters XBridgeTM C18 column (250 mm x 4.6 mm I.D., 5μm), with mobile phase consisted of potassium phosphate buffer (0.05 M, pH 3.2): acetonitrile (86:14, v/v), and UV detection set at 303 nm. The analyses of MTX content by the UV method were also accomplished at 303 nm, using 0.1 M sodium hydroxide as diluent. The measurements were linearly correlated with concentration for both methods in the 1 - 30 μg/mL range (r > 0.9999). The specificity tests showed that there was no interference of the NP components on the quantitative analyses. Precision (repeatability and intermediate precision) was demonstrated by a relative standard deviation lower than 1.5%, whereas the accuracy was assessed by the recovery of MTX from sample matrices, given mean value of ~99%. The proposed methods were applied for the analyses of MTX in different batches of NPs, and the results showed non-significant differences (p > 0.05) between the values obtained with both methodologies. Moreover, the RP-LC method was successfully used to determine the drug entrapment efficiency, and to quantify MTX during in vitro release assays and photolytic degradation studies. In conclusion, the validated methods are suitable to assay MTX in pH-sensitive CS-NPs without any interference from the polymer or surfactant.Pharma Publisher2016201620142016info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersion9 p.application/pdfhttps://hdl.handle.net/2445/97209Articles publicats en revistes (Bioquímica i Fisiologia)reponame:Recercat. Dipósit de la Recerca de Catalunyainstname:Varias* (Consorci de Biblioteques Universitáries de Catalunya, Centre de Serveis Científics i Acadèmics de Catalunya)InglésReproducció del document publicat a: http://dx.doi.org/10.14205/2309-4435.2014.02.02.3Journal of Applied Biopharmaceutics and Pharmacokinetics , 2014, vol. 2, num. 2, p. 59-67http://dx.doi.org/10.14205/2309-4435.2014.02.02.3cc-by-nc (c) Nogueira D.R. et al., 2014http://creativecommons.org/licenses/by-nc/3.0/esinfo:eu-repo/semantics/openAccessoai:recercat.cat:2445/972092026-05-29T05:05:01Z
dc.title.none.fl_str_mv Determination of Methotrexate in pH-Sensitive Chitosan Nanoparticles by Validated RP-LC and UV Spectrophotometric Methods
title Determination of Methotrexate in pH-Sensitive Chitosan Nanoparticles by Validated RP-LC and UV Spectrophotometric Methods
spellingShingle Determination of Methotrexate in pH-Sensitive Chitosan Nanoparticles by Validated RP-LC and UV Spectrophotometric Methods
Nogueira, Daniele R.
Quitosan
Nanopartícules
Medicaments antineoplàstics
Metotrexat
Agents tensioactius
Cromatografia
Espectroscòpia
Chitosan
Nanoparticles
Antineoplastic agents
Methotrexate
Surface active agents
Chromatography
Spectrum analysis
title_short Determination of Methotrexate in pH-Sensitive Chitosan Nanoparticles by Validated RP-LC and UV Spectrophotometric Methods
title_full Determination of Methotrexate in pH-Sensitive Chitosan Nanoparticles by Validated RP-LC and UV Spectrophotometric Methods
title_fullStr Determination of Methotrexate in pH-Sensitive Chitosan Nanoparticles by Validated RP-LC and UV Spectrophotometric Methods
title_full_unstemmed Determination of Methotrexate in pH-Sensitive Chitosan Nanoparticles by Validated RP-LC and UV Spectrophotometric Methods
title_sort Determination of Methotrexate in pH-Sensitive Chitosan Nanoparticles by Validated RP-LC and UV Spectrophotometric Methods
dc.creator.none.fl_str_mv Nogueira, Daniele R.
Macedo, Letícia B.
Scheeren, Laís E.
Mitjans Arnal, Montserrat
Infante Martínez-Pardo, Ma. Rosa
Rolim, Clarice M. B.
Vinardell Martínez-Hidalgo, Ma. Pilar
author Nogueira, Daniele R.
author_facet Nogueira, Daniele R.
Macedo, Letícia B.
Scheeren, Laís E.
Mitjans Arnal, Montserrat
Infante Martínez-Pardo, Ma. Rosa
Rolim, Clarice M. B.
Vinardell Martínez-Hidalgo, Ma. Pilar
author_role author
author2 Macedo, Letícia B.
Scheeren, Laís E.
Mitjans Arnal, Montserrat
Infante Martínez-Pardo, Ma. Rosa
Rolim, Clarice M. B.
Vinardell Martínez-Hidalgo, Ma. Pilar
author2_role author
author
author
author
author
author
dc.subject.none.fl_str_mv Quitosan
Nanopartícules
Medicaments antineoplàstics
Metotrexat
Agents tensioactius
Cromatografia
Espectroscòpia
Chitosan
Nanoparticles
Antineoplastic agents
Methotrexate
Surface active agents
Chromatography
Spectrum analysis
topic Quitosan
Nanopartícules
Medicaments antineoplàstics
Metotrexat
Agents tensioactius
Cromatografia
Espectroscòpia
Chitosan
Nanoparticles
Antineoplastic agents
Methotrexate
Surface active agents
Chromatography
Spectrum analysis
description Nanotechnology-based drug delivery systems are in constant development and, therefore, it is of great importance to have rapid, efficient and accurate analytical methodology to quantify the encapsulated drugs. Here, simple and fast methods, by reversed-phase liquid chromatography (RP-LC) and UV spectrophotometry, were developed and validated for the determination of methotrexate (MTX) in pH-sensitive chitosan nanoparticles (CS-NPs). NPs were prepared using a modified ionotropic complexation process, in which was included a surfactant derived from Nα,Nε-dioctanoyl lysine with an inorganic sodium counterion. The RP-LC method was carried out on a Waters XBridgeTM C18 column (250 mm x 4.6 mm I.D., 5μm), with mobile phase consisted of potassium phosphate buffer (0.05 M, pH 3.2): acetonitrile (86:14, v/v), and UV detection set at 303 nm. The analyses of MTX content by the UV method were also accomplished at 303 nm, using 0.1 M sodium hydroxide as diluent. The measurements were linearly correlated with concentration for both methods in the 1 - 30 μg/mL range (r > 0.9999). The specificity tests showed that there was no interference of the NP components on the quantitative analyses. Precision (repeatability and intermediate precision) was demonstrated by a relative standard deviation lower than 1.5%, whereas the accuracy was assessed by the recovery of MTX from sample matrices, given mean value of ~99%. The proposed methods were applied for the analyses of MTX in different batches of NPs, and the results showed non-significant differences (p > 0.05) between the values obtained with both methodologies. Moreover, the RP-LC method was successfully used to determine the drug entrapment efficiency, and to quantify MTX during in vitro release assays and photolytic degradation studies. In conclusion, the validated methods are suitable to assay MTX in pH-sensitive CS-NPs without any interference from the polymer or surfactant.
publishDate 2014
dc.date.none.fl_str_mv 2014
2016
2016
2016
dc.type.none.fl_str_mv info:eu-repo/semantics/article
info:eu-repo/semantics/publishedVersion
format article
status_str publishedVersion
dc.identifier.none.fl_str_mv https://hdl.handle.net/2445/97209
url https://hdl.handle.net/2445/97209
dc.language.none.fl_str_mv Inglés
language_invalid_str_mv Inglés
dc.relation.none.fl_str_mv Reproducció del document publicat a: http://dx.doi.org/10.14205/2309-4435.2014.02.02.3
Journal of Applied Biopharmaceutics and Pharmacokinetics , 2014, vol. 2, num. 2, p. 59-67
http://dx.doi.org/10.14205/2309-4435.2014.02.02.3
dc.rights.none.fl_str_mv cc-by-nc (c) Nogueira D.R. et al., 2014
http://creativecommons.org/licenses/by-nc/3.0/es
info:eu-repo/semantics/openAccess
rights_invalid_str_mv cc-by-nc (c) Nogueira D.R. et al., 2014
http://creativecommons.org/licenses/by-nc/3.0/es
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv 9 p.
application/pdf
dc.publisher.none.fl_str_mv Pharma Publisher
publisher.none.fl_str_mv Pharma Publisher
dc.source.none.fl_str_mv Articles publicats en revistes (Bioquímica i Fisiologia)
reponame:Recercat. Dipósit de la Recerca de Catalunya
instname:Varias* (Consorci de Biblioteques Universitáries de Catalunya, Centre de Serveis Científics i Acadèmics de Catalunya)
instname_str Varias* (Consorci de Biblioteques Universitáries de Catalunya, Centre de Serveis Científics i Acadèmics de Catalunya)
reponame_str Recercat. Dipósit de la Recerca de Catalunya
collection Recercat. Dipósit de la Recerca de Catalunya
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repository.mail.fl_str_mv
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