Stability-indicating thin-layer chromatographic method for determination of darunavir in complex darunavir-beta-cyclodextrin in the presence of its degradation products

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dc.contributor.authorKogawa, Ana Carolina [UNESP]
dc.contributor.authorMendonca, Jaqueline Nakau
dc.contributor.authorLopes, Norberto Peporine
dc.contributor.authorSalgado, Hérida Regina Nunes [UNESP]
dc.contributor.institutionUniversidade Estadual Paulista (Unesp)
dc.contributor.institutionUniversidade de São Paulo (USP)
dc.date.accessioned2014-12-03T13:11:44Z
dc.date.available2014-12-03T13:11:44Z
dc.date.issued2014-06-07
dc.description.abstractDarunavir (DRV), a protease inhibitor used in the treatment of HIV infection, presents low water solubility and poor bioavailability. Therefore, the complexation of DRV with beta-cyclodextrin (beta-CD) was performed. This drug is not described in official compendiums. A simple, selective and inexpensive stability-indicating thin-layer chromatographic (TLC) method for the determinations of DRV in complex DRV-beta-CD and its degradation products was developed. The TLC method employs aluminum plates precoated with silica gel 60(F-254) as the stationary phase and purified water and methanol, 70 : 30 (v/v) adjusted to pH 2.4 with glacial acetic acid as the solvent system to provide spots for DRV (R-f = 0.66) and its degradation products in acidic (R-f = 0.73 and 0.76), basic (R-f = 0.53) and oxidative (R-f = 0.71, 0,75 and 0.84) media. The chromatogram was visualized in a UVA chamber at 365 nm. HPLC analysis was performed on a Waters HPLC system, Phenomenex CN Luna (250 x 4.6 mm) column and mobile phase consisting of water + 0.1% glacial acetic acid and acetonitrile + 0.1% glacial acetic acid in the ratio 60 : 40 (v/v) at a flow rate of 1.0 mL min(-1) and 268 nm for the separation of DRV (t(R) = 7.3) and its degradation products in acidic (t(R) = 5.1 and 6.7 min), basic (t(R) = 7.8 min) and oxidative (t(R) = 5.1, 5.5 and 6.7 min) media. DRV-beta-CD was subjected to acid and alkali hydrolysis and oxidation and analyzed by the proposed methods in the presence of its degradation products, which were identified by LC-MS. As the methods could separate DRV from the degradation products, these techniques can be employed as indicative stability methods and can be effectively applied in quality control of DRV complexed to beta-CD.en
dc.description.affiliationUniv Estadual Paulista, Dept Drugs & Pharmaceut, Sch Pharmaceut Sci, UNESP, Sao Paulo, Brazil
dc.description.affiliationUniv Sao Paulo, Fac Pharmaceut Sci Ribeirao Preto, Dept Chem & Phys, Ctr Res Nat & Synthet Prod, BR-14049 Ribeirao Preto, Brazil
dc.description.affiliationUnespUniv Estadual Paulista, Dept Drugs & Pharmaceut, Sch Pharmaceut Sci, UNESP, Sao Paulo, Brazil
dc.description.sponsorshipConselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
dc.description.sponsorshipFundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
dc.description.sponsorshipCoordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
dc.description.sponsorshipPADC/FCF/UNESP (Araraquara, Brazil)
dc.format.extent3689-3693
dc.identifierhttp://dx.doi.org/10.1039/c4ay00248b
dc.identifier.citationAnalytical Methods. Cambridge: Royal Soc Chemistry, v. 6, n. 11, p. 3689-3693, 2014.
dc.identifier.doi10.1039/c4ay00248b
dc.identifier.issn1759-9660
dc.identifier.urihttp://hdl.handle.net/11449/113472
dc.identifier.wosWOS:000336820300022
dc.language.isoeng
dc.publisherRoyal Soc Chemistry
dc.relation.ispartofAnalytical Methods
dc.relation.ispartofjcr2.073
dc.relation.ispartofsjr0,619
dc.rights.accessRightsAcesso restrito
dc.sourceWeb of Science
dc.titleStability-indicating thin-layer chromatographic method for determination of darunavir in complex darunavir-beta-cyclodextrin in the presence of its degradation productsen
dc.typeArtigo
dcterms.rightsHolderRoyal Soc Chemistry
unesp.campusUniversidade Estadual Paulista (Unesp), Faculdade de Ciências Farmacêuticas, Araraquarapt

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