Título: | SELECTIVE DETERMINATION OF FLUORQUINOLONES FOR CELLULOSE SURFACE ROOMTEMPERATURE PHOSPHORIMETRY WHITH THORIUM NITRATE | ||||||||||||||||||||||||||||||||||||||||||||
Autor: |
ILFRAN DA SILVA NAVA JUNIOR |
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Colaborador(es): |
RICARDO QUEIROZ AUCELIO - Orientador PERCIO AUGUSTO MARDINI FARIAS - Coorientador |
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Catalogação: | 16/OUT/2007 | Língua(s): | PORTUGUESE - BRAZIL |
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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. |
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Referência(s): |
[pt] https://www.maxwell.vrac.puc-rio.br/projetosEspeciais/ETDs/consultas/conteudo.php?strSecao=resultado&nrSeq=10720&idi=1 [en] https://www.maxwell.vrac.puc-rio.br/projetosEspeciais/ETDs/consultas/conteudo.php?strSecao=resultado&nrSeq=10720&idi=2 |
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DOI: | https://doi.org/10.17771/PUCRio.acad.10720 | ||||||||||||||||||||||||||||||||||||||||||||
Resumo: | |||||||||||||||||||||||||||||||||||||||||||||
In this work, analytical methods based on solid surface
room-temperature
phosphorimetry were developed aiming the selective
determination of
fluorquinolones. More spectilly, thorium nitrate was
evaluated as
phosphorescence inducer aiming the sequential
determination of norfloxacin
(NOR) and levofloxacin (LEV), selective determination of
NOR in presence of
ciprofloxacin (CIP), as well as the selective
determination of CIP in the presence
gatifloxacin (GAT) or moxifloxacin (MOX). In order to
that, the phosphorescence
induced by thorium nitrate was compared with the ones
achieved using other
traditionally employed heavy atom enhancers in solid
surface room-temperature
phosphorimetry (SSRTP). Univariated studies were made in
order to evaluate the
effect of the amounts of heavy atom salt and surface
modifier present in the
substrate as well as the influence of the pH of the
analyte carrier solution. The
interaction among these factors were also studied through
experimental factorial
desings (23). After the definition of the analytical
strategy to be employed,
analytical methods were developed for the determination of
NOR, LEV and CIP in
simulated mistures and analyte spiked urine without
employing any procedure to
physically separate the analyte from the others components
of the sample. In
order to do that, the use of syncronized scanning was
fundamental. The
analytical figures of merit achieved using thorium nitrate
and cadmium acetate
(heave atom inducer already reported in the literature for
fluorquinolones) were
campared. In both cases, linear analytical responses in
function of the amount of
analyted present in the substrate were achieved (R2>0,99).
Good repetitivity of
results and sensibility (evaluated through the estimation
of the limits of detection
and quantification) were in the ng order. When testing
pharmaceutical
formulations and spiked urine, the use of Th(NO3)4 showed
clear advantage over
Cd(OAc)2, allowing the sequential determination of NOR/LEV
and the selective
determination of NOR in the presence of CIP. The selective
determination of
NOR using Th(NO3)4 could be made for mixtures containing
up to five times more LEV or CIP in molar proportion. For
the developed method aiming the
determination of CIP in mistures containing GAT, Th(NO3)4
was found to be more
adequate heavy atom enhancer than Cd(OAc)2. The method was
free from
interferences for samples containing two times more GAT
than CIP (in molar
proportion). However, interferences observed for mixtures
containing higher
amounts of GAT could be easily corrected by the using of
the standard addition
method for quantification. In mixtures containing CIP and
MOX, the developed
method using Th(NO3)4 was suitable for mixtures containing
equimolar
proportions of these two fluorquinolones. Spectral
interferences were observed
for higher amounts of MOX. Such interference could not be
resolved due to close
(lambda) values characteristic for the two FQs. However,
for the
method using
Cd(OAc)2 in mixtures containing CIP/MOX in molar
proportion more them 1:2
only non spectral interferences were observed, but this
interferences can be
corrected by the use of proper calibration strategy. This
was the only situation
where Cd(OAc)2 demonstrate better results than Th(NO3)4.
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