Desenvolvimento de nova fase extratora monolítica para extração sortiva em ponteira descartável, aplicada à análise de dexametasona em liquido sinovial sintético

• Ano de defesa: 2019
• Autor(a) principal: Machado, Lucas Santos
• Orientador(a): Chaves, Andrea Rodrigues
• Banca de defesa: Chaves, Andrea Rodrigues, Sgobbi, Lívia Flório, Teixeira, Leonardo de Souza
• Tipo de documento: Dissertação
• Tipo de acesso: Acesso aberto
• Idioma: por
• Instituição de defesa: Universidade Federal de Goiás
• Programa de Pós-Graduação: Programa de Pós-graduação em Química (IQ)
• Departamento: Instituto de Química - IQ (RG)
• País: Brasil
• Palavras-chave em Português: Preparo de amostra; DPX; Polímero monolítico; Dexametasona; Líquido sinovial
• Palavras-chave em Inglês: Sample preparation; Monolithic polime; Dexamethasone; Synovial liquid
• Área do conhecimento CNPq: CIENCIAS EXATAS E DA TERRA::QUIMICA::QUIMICA ANALITICA::METODOS OTICOS DE ANALISE
• Link de acesso: http://repositorio.bc.ufg.br/tede/handle/tede/11178

Disposable pipette extraction (DPX) is a sample preparation techniques which contains an extractive phase in a conventional micropipette tip (1 or 5 mL). The first commercially available extractor phase used polymer modified C18 particles. Since then, different materials have been evaluated as sorbents, among which stand out the monolithic polymers, which consist of a continuous means of separation giving high permeability to the phase. The determination of concentrations of dexamethasone in synovial fluid presents an analytical challenge, considering the low concentrations evaluated and the number of endogenous compounds present in this matrix. Therefore, the present study employed styrene and divinylbenzene-based monolithic polymers as the extraction phase for DPX extraction of dexamethasone in synthetic synovial fluid. The monoliths were synthesized by mass polymerization and emulsion, the latter was modified by pyrrole, in both cases a micropipette tip was used as a mold. The monolithis were characterized by Fourier transformed infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and desorption and nitrogen absorption. The synthesized pipette tips were evaluated for DPX extraction of dexamethasone in synthetic synovial fluid samples, followed by ultraviolet detector liquid chromatography (HPLC-UV) analysis and the pyrrole modified pipette tip exhibited higher extraction efficiency. Using factorial design 24, considering the main variables of the DPX method, the optimal analysis condition for dexamethasone extraction in the analyzed matrix was determined. Some method figures such as detection limit 5 ng mL-1, quantitation limit 10 ng mL-1, precision and accuracy, were evaluated to prove the effectiveness of the proposed method for dexamethasone extraction by observing parameters befitting with those required by ANVISA. Thus, the developed DPX / HPLC-UV method proved to be a promising tool for the determination of dexamethasone in synovial fluid.