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Development of MEPS–UHPLC/PDA methodology for the quantification of clozapine, risperidone and their major active metabolites in human urine

2015Journal article Restricted access
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dc.contributor.authorGonçalves, João L.
dc.contributor.authorAlves, Vera L.
dc.contributor.authorConceição, Carlota J.F.
dc.contributor.authorTeixeira, Helena M.
dc.contributor.authorCâmara, José S.
dc.date.accessioned2019-07-22T14:03:26Z
dc.date.available2019-07-22T14:03:26Z
dc.date.issued2015
dc.description.abstractA new, fast and reliable methodology using a digitally controlled microextraction by packed sorbent (MEPS), followed by ultrahigh pressure liquid chromatography (UHPLC) separation combined with a photodiode array (PDA) detection, has been developed and validated for the simultaneous determination of clozapine and risperidone, and their active metabolites, in urine samples. Important parameters affecting MEPS performance, including type of sorbent material (C2, C8, C18, SIL, M1, R-AX, R-CX, PGC, PEP, HLB-DVB and H-DVB), elution solvent system, number of extraction cycles, sample volume, elution volume, and sample pH, were evaluated. The optimal experimental conditions involved the loading of 500 μl of sample through a C18 sorbent in a five extraction cycles and in a short time period (5 min for the entire sample preparation step). The obtained extract was analyzed by UHPLC, using a binary mobile phase, composed of aqueous 0.1% formic acid and methanol in the gradient elution mode (10 min total analysis). Good results were obtained under the optimized conditions, in terms of linearity with correlation coefficients (r2) values higher than 0.9986. Low detection limits, ranging between 0.052 and 0.055 μg ml− 1 were achieved, whereas the lowest quantification limit was 0.1 μg ml− 1, corresponding to the lowest concentration of the standard curve. Satisfactory results were found with accuracy values ranging from 83% to 116%, and with precision results from 2.65% to 18%. Recoveries ranged between 76% and 96%, which was in agreement with results reported by other studies.pt_PT
dc.description.versioninfo:eu-repo/semantics/publishedVersionpt_PT
dc.identifier.citationGonçalves, J. L., Alves, V. L., Conceição, C. J., Teixeira, H. M., & Câmara, J. S. (2015). Development of MEPS–UHPLC/PDA methodology for the quantification of clozapine, risperidone and their major active metabolites in human urine. Microchemical Journal, 123, 90-98.pt_PT
dc.identifier.doi10.1016/j.microc.2015.05.016pt_PT
dc.identifier.issn0026-265X
dc.identifier.urihttp://hdl.handle.net/10400.13/2496
dc.language.isoengpt_PT
dc.publisherElsevierpt_PT
dc.subjectAntipsychoticspt_PT
dc.subjectClozapinept_PT
dc.subjectRisperidonept_PT
dc.subjectMicroextraction by packed sorbentpt_PT
dc.subjectUltra high pressure liquid chromatographypt_PT
dc.subject.pt_PT
dc.subjectFaculdade de Ciências Exatas e da Engenhariapt_PT
dc.subjectCentro de Química da Madeira
dc.titleDevelopment of MEPS–UHPLC/PDA methodology for the quantification of clozapine, risperidone and their major active metabolites in human urinept_PT
dc.typejournal article
dspace.entity.typePublication
oaire.citation.endPage98pt_PT
oaire.citation.startPage90pt_PT
oaire.citation.titleMicrochemical Journalpt_PT
oaire.citation.volume123pt_PT
person.familyNameGonçalves
person.familyNameAlves
person.familyNameCâmara
person.givenNameJoão
person.givenNameVera
person.givenNameJosé
person.identifierG-3003-2013
person.identifier.ciencia-id8C14-3188-9E44
person.identifier.ciencia-idE515-0AFA-CB1D
person.identifier.ciencia-id481C-08CE-90E5
person.identifier.orcid0000-0002-1265-6686
person.identifier.orcid0000-0002-1485-6032
person.identifier.orcid0000-0003-1965-3151
person.identifier.ridC-1348-2019
person.identifier.scopus-author-id52163735200
person.identifier.scopus-author-id55792994000
person.identifier.scopus-author-id10140393000
rcaap.rightsrestrictedAccesspt_PT
rcaap.typearticlept_PT
relation.isAuthorOfPublication7971c475-3f08-4462-96b1-79e96c9615a4
relation.isAuthorOfPublication4d9a888c-6c61-448b-985a-ec64eadac0b2
relation.isAuthorOfPublicatione10d78be-e547-4d25-92b5-06a997ed78da
relation.isAuthorOfPublication.latestForDiscovery7971c475-3f08-4462-96b1-79e96c9615a4

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