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Coleção Digital

Avançada


Estatísticas | Formato DC |



Título: ANALYTICAL METHODS BASED ON PHOTOCHEMICALLY INDUCED FLUORESCENCE: SPECTROFLUORIMETRIC AND CHROMATOGRAPHIC APPLICATIONS FOR THE DETERMINATION OF TETRABENAZINE, AMITRIPTYLINE AND VARENICLINE
Autor: ANA CATALINA PALACIOS OSORIO
Instituição: PONTIFÍCIA UNIVERSIDADE CATÓLICA DO RIO DE JANEIRO - PUC-RIO
Colaborador(es):  RICARDO QUEIROZ AUCELIO - ADVISOR
ALESSANDRA LICURSI MAIA CERQUEIRA DA CUNHA - CO-ADVISOR

Nº do Conteudo: 56789
Catalogação:  27/12/2021 Idioma(s):  PORTUGUESE - BRAZIL
Tipo:  TEXT Subtipo:  THESIS
Natureza:  SCHOLARLY PUBLICATION
Nota:  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.
Referência [pt]:  https://www.maxwell.vrac.puc-rio.br/colecao.php?strSecao=resultado&nrSeq=56789@1
Referência [en]:  https://www.maxwell.vrac.puc-rio.br/colecao.php?strSecao=resultado&nrSeq=56789@2
Referência DOI:  https://doi.org/10.17771/PUCRio.acad.56789

Resumo:
Photochemical derivatization was employed to induce or amplify the fluorescence from three substances with pharmacological activities: tetrabenazine (TBZ); amitriptyline (AMT) and varenicline (VRN). The substantial fluorescence enhancement after UV irradiation allowed the development of methods based on spectrofluorimetry for TBZ, AMT and VRN. The approach was also evaluated in high performance liquid chromatography (HPLC) with fluorimetric detection for the determination of the concentration AMT and VRN in drugs or in biological matrices. For the determination of TBZ, 60 min of UV irradiation of the analyte prepared in NaOH (0.45 mol L-1) allowed its indirect quantification using spectrofluorimetry, with a limit of detection (LOD) of 1.4 x 10-8 mol L-1 and a linear response up to 1.0 x 10-5 mol L-1. Pre-concentration using solid phase extraction improved the LOD in one order of magnitude. The spectrofluorimetric method was applied for the determination of TBZ in a commercial drug, with recoveries between 88 and 95%. TBZ was also determined in analyte fortified saliva at a concentration near the limit of quantitation (LOQ) with recoveries greater than 87%. Studies using plasma desorption mass spectrometry with a 252Cf source, indicated that the photoderivatives of TBZ were obtained through a Norrish Type I and II TBZ photolysis. For the determination of AMT, two photochemical derivatization approaches allowed the determination of the substance by spectrofluorimetry. The approach using HPLC coupled to fluorescence detection was also tested. For the spectrofluorimetric method, the derivatization was achieved after 60 min of UV exposure of a solution of AMT prepared in HCl 0.027 mol L-1. The linear response of the method was up to 1.0 x 10-5 mol L-1 of AMT, with a LOD of 4.8 x 10-8 mol L-1. For the chromatographic method, the derivatization process was adjusted (30 min of UV irradiation in phosphate buffer, pH 3) in order to adapt the reaction for HPLC. The method allowed an LOD of 6.0 x10-9 mol L-1 with a linear range up to 2.5 x 10-6 mol L-1 of AMT. The determination of AMT in drugs and in a pharmacopeial reference material was performed, with recoveries between 94 and 105% for the fluorimetric method and between 99 and 111% using HPLC. The analysis of human plasma was also made using AMT (1.0 x 10-6 mol L-1) fortified samples. The fluorescent photoderivatives were separated and identified by GC-MS, which allowed the proposal of a photolysis mechanism of AMT. For the determination of VRN, the photochemical derivatization in basic medium allowed the determination of the substance by spectrofluorimetry. The derivatization of VRN, performed by exposing the analyte to the UV during 23 minutes in NaOH 0.64 mol L-1, allowed a LOD of 1.5 x10-8 mol L-1 and a linear range extending up to 1.0 x10-6 mol L-1. The derivatization condition were also adapted for the determination of the analyte using HPLC with fluorimetric detection, by irradiating VRN for 10 min in borate buffer (0.01 mol L-1 pH 10). Both methods were applied for the determination of VRN in a commercial drug, with recoveries between 93 and 102%. For all the developed methods, a simplified metrological evaluation was performed, considering the most relevant sources of uncertainty during the measurement process of the analytes studied in this thesis: solution preparation, intra and inter-day precision and the analytical curve. The uncertainty sources for each of the proposed methods were estimated in three different concentrations within the linear range. Measurement uncertainty estimations were between 5.8 and 36% of the nominal concentration in the concentrations near the LOQ and between 3.1 and 16% in the concentrations within the linear range of the methods. Safer, energetically efficient procedures with solvent reduction and without the use of toxic reagents were proposed, in agreement to green chemistry principles.

Descrição Arquivo
COVER, ACKNOWLEDGEMENTS, RESUMO, ABSTRACT, SUMMARY AND LISTS  PDF
CHAPTER 1  PDF
CHAPTER 2  PDF
CHAPTER 3  PDF
CHAPTER 4  PDF
CHAPTER 5  PDF
CHAPTER 6  PDF
CHAPTER 7  PDF
REFERENCES  PDF
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