Analysis of fluoxetine and norfluoxetine in human plasma by HPLC-UV using a high purity C18 silica-based SPE sorbent

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dc.contributor.authorNazario, Carlos Eduardo Domingues
dc.contributor.authorLima Gomes, Paulo Clairmont Feitosa de [UNESP]
dc.contributor.authorLancas, Fernando Mauro
dc.contributor.institutionUniversidade Estadual Paulista (Unesp)
dc.contributor.institutionUniversidade de São Paulo (USP)
dc.date.accessioned2015-05-15T13:30:21Z
dc.date.available2015-05-15T13:30:21Z
dc.date.issued2014
dc.description.abstractThis paper reports on the development and validation of a simple and sensitive method that uses solid phase extraction (SPE) and liquid chromatography with ultraviolet detection to analyze fluoxetine (FLX) and norfluoxetine (NFLX) in human plasma samples. A lab-made C18 SPE phase was synthesized by using a sol–gel process employing a low-cost silica precursor. This sorbent was fully characterized by nuclear magnetic resonance (NMR), Fourier-transform infrared spectroscopy (FT-IR), and scanning electron microscopy (SEM) to check the particles' shape, size and C18 functionalization. The lab-made C18 silica was used in the sample preparation step of human plasma by the SPE-HPLC-UV method. The method was validated in the 15 to 500 ng mL 1 range for both FLX and NFLX using a matrix matched curve. Detection limits of 4.3 and 4.2 ng mL 1 were obtained for FLX and NFLX, respectively. The repeatability and intermediary precision achieved varied from 7.6 to 15.0% and the accuracy ranged from 14.9 to 9.1%. The synthesized C18 sorbent was compared to commercial C18 sorbents. The average recoveries were similar (85–105%), however the lab-made C18 silica showed fewer interfering peaks in the chromatogram. After development and validation, the method using the lab-made C18 SPE was applied to plasma samples of patients under FLX treatment (n ¼ 6). The concentrations of FLX and NFLX found in the samples varied from 46.8–215.5 and 48.0–189.9 ng mL 1 , respectively.en
dc.description.affiliationUniversidade Estadual Paulista Júlio de Mesquita Filho, Instituto de Química de Araraquara, Araraquara, Rua Professor Francisco Degni, Departamento de Química Analítica, Jardim Quitandinha, CEP 14800060, SP, Brasil
dc.description.affiliationUnespUniversidade Estadual Paulista Júlio de Mesquita Filho, Instituto de Química de Araraquara, Araraquara, Rua Professor Francisco Degni, Departamento de Química Analítica, Jardim Quitandinha, CEP 14800060, SP, Brasil
dc.format.extent4181-4187
dc.identifierhttp://pubs.rsc.org/en/Content/ArticleLanding/2014/AY/c4ay00117f#!divAbstract
dc.identifier.citationAnalytical Methods, v. 6, n. 12, p. 4181-4187, 2014.
dc.identifier.doi10.1039/c4ay00117f
dc.identifier.issn1759-9660
dc.identifier.lattes49857977635051
dc.identifier.urihttp://hdl.handle.net/11449/123523
dc.language.isoeng
dc.relation.ispartofAnalytical Methods
dc.relation.ispartofjcr2.073
dc.relation.ispartofsjr0,619
dc.rights.accessRightsAcesso restrito
dc.sourceCurrículo Lattes
dc.titleAnalysis of fluoxetine and norfluoxetine in human plasma by HPLC-UV using a high purity C18 silica-based SPE sorbenten
dc.typeArtigo
unesp.author.lattes49857977635051
unesp.campusUniversidade Estadual Paulista (Unesp), Instituto de Química, Araraquarapt

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