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Estatística
Título: DEVELOPMENT AND METROLOGICAL VALIDATION OF A HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR THE QUANTIFICATION OF CYCLOFENIL AFTER PHOTOCHEMICAL DERIVATIZATION
Autor: JUAN JOSE GARCIA ANTONIO
Colaborador(es): ELISABETH COSTA MONTEIRO - Orientador
RICARDO QUEIROZ AUCELIO - Coorientador
ALESSANDRA LICURSI MAIA CERQUEIRA DA CUNHA - Coorientador
Catalogação: 22/OUT/2013 Língua(s): PORTUGUESE - BRAZIL
Tipo: TEXT Subtipo: THESIS
Notas: [pt] Todos os dados constantes dos documentos são de inteira responsabilidade de seus autores. Os dados utilizados nas descrições dos documentos estão em conformidade com os sistemas da administração da PUC-Rio.
[en] All data contained in the documents are the sole responsibility of the authors. The data used in the descriptions of the documents are in conformity with the systems of the administration of PUC-Rio.
Referência(s): [pt] https://www.maxwell.vrac.puc-rio.br/projetosEspeciais/ETDs/consultas/conteudo.php?strSecao=resultado&nrSeq=22176&idi=1
[en] https://www.maxwell.vrac.puc-rio.br/projetosEspeciais/ETDs/consultas/conteudo.php?strSecao=resultado&nrSeq=22176&idi=2
DOI: https://doi.org/10.17771/PUCRio.acad.22176
Resumo:
Cyclofenil is an anti-estrogen used in treatments of ovarian disorders. On the other hand, its effect in men results in the increasing of muscle mass, being its use, by male athletes, banned by the World Anti-Doping Code established by World Anti-Doping Agency. Absorption and fluorescence spectrophotometries allow direct or indirect quantification of cyclofenil, however, they are not suitable for the analysis of complex samples. This work proposes the development of a method based on high performance liquid chromatography to determine cyclofenil using photochemical induced fluorescence detection. The separation using isocratic elution (10 mmol/L(-1) borate buffer at pH 10/methanol (60/40 per cent v/v), and column C18 maintained at 35 degrees celsius. After exposing cyclofenil to the UV, fluorescent photoderivatives were formed, as indicated in the literature, with the photoderivative with the retention time of 2.7 min used for quantitative purposes since it is stable for over 96 h after the photoderivatization procedure. The detection limit was 6.6 x 10(-8) mol/L(-1) and the limit of quantification was 7.3 x 10(-7) mol/L(-1). The linear response range extended up to 5 x 10(-5) mol/L(-1) (as cyclofenil). Recoveries in pharmaceutical formulations were between 94 and 105 per cent. The results indicated that the homogeneity and stability of cyclofenil tablets are satisfactory. The uncertainty sources that present the greatest contributions to the measurement uncertainty were the ones associated with the preparation of the solutions and the analytical curve.
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