Desenvolvimento de métodos analíticos limpos para determinações forenses: chumbo em resíduos de disparo e furosemida em doping
Carregando...
Arquivos
Data
2012-01-17
Autores
Luiz, Vitor Hugo Marques [UNESP]
Título da Revista
ISSN da Revista
Título de Volume
Editor
Universidade Estadual Paulista (Unesp)
Resumo
Este projeto descreve o desenvolvimento de um método analítico para a determinação quantitativa de furosemida em amostras de urina, o desenvolvimento de um novo método de coleta e de análise de resíduos de armas de fogo para a posterior determinação quantitativa de chumbo coletado nas mãos dos atiradores, nos lugares de impacto e nos cartuchos de munição. O método para determinação de chumbo também foi aplicado para amostras de cachaças. Atualmente sabe-se que a realidade dos laboratórios forenses é muito diferente daquelas mostradas nas séries e filmes. São muito poucos aqueles que disponibilizam de equipamentos mais sensíveis que são, consequentemente, mais caros. Visto este problema, o presente trabalho visa desenvolver métodos simples, rápidos, de baixo custo, repetitíveis e mais limpos utilizando a técnica da espectroscopia de reflectância difusa. Os métodos desenvolvidos consistem na reação da furosemida com o regente cromogênico cloreto de ferro(III) (FeCl3) em meio micelar de brometo de dodeciltrimetilamônio (DTAB) e na reação do íon chumbo(II) (Pb2+) com rodizonato de sódio (ROD) em meio micelar de dodecil sulfato de sódio (SDS), cujas concentrações foram otimizadas por planejamentos quimiométricos. As reações foram realizadas na forma de spot test, utilizando papel de filtro qualitativo da marca Whatman como suporte sólido, envolvendo a formação de um produto colorido em 477 nm para a furosemida e 545 nm para o chumbo. As curvas analíticas foram construídas a partir de soluções padrão de furosemida (FUR) e de Pb2+. O Limite de Detecção (LD) e o Limite de Quantificação (LQ) foram, respectivamente, 0,49 e 1,62 mmol L-1 para a furosemida e 1,12 e 3,75 ppm para o chumbo, de acordo com o recomendado pela IUPAC. Os métodos propostos foram aplicados...
This project describes the development of an analytical method for the quantitative determination of furosemide in urine samples, the development of a new collection and analysis method of gunshot residues and the subsequent quantitative determination of the lead collected from the shooter´s hand, in the impact sites and in the rounds of ammunition. The method for lead detection was also applied for cachaça. Nowadays it is known that the reality in forensic laboratories is very different of that seen in series and movies. There are few laboratories which have more sensible equipments, being more expensive. Having in mind this problem, the present work aims the development of methods that are simple, fast, cheap, repeatable and cleaner using diffuse reflectance spectroscopy. The developed methods consists in the reaction of furosemide with the chromogenic reagent iron(III) chloride (FeCl3) in a micellar medium of dodecyltrimethylammonium bromide (DTAB) and in the reaction of lead ion (Pb2+) with sodium rhodizonate (ROD) in a micellar medium of sodium dodecyl sulfate (SDS), which concentrations were optimized by chemometrics. The reactions were realized as spot test using Whatman qualitative filter paper as a solid support, involving the formation of a colored product in 477 nm for furosemide and 545 nm for lead ion. The analytical curves were constructed from standard solutions of furosemide and lead. The Limit of Detection (LoD) and the Limit of Quantification (LoQ) were, respectively, 0,49 and 1,62 mmol L-1 for furosemide and 1,12 and 3,75 ppm for lead, accordingly to the recommendations of IUPAC. The proposed methods were applied for the determination of furosemide in synthetic and human urine and for the determination of lead in gunshot residues (GSRs) and in commercial sugar cane brandy, with the... (Complete abstract click electronic access below)
This project describes the development of an analytical method for the quantitative determination of furosemide in urine samples, the development of a new collection and analysis method of gunshot residues and the subsequent quantitative determination of the lead collected from the shooter´s hand, in the impact sites and in the rounds of ammunition. The method for lead detection was also applied for cachaça. Nowadays it is known that the reality in forensic laboratories is very different of that seen in series and movies. There are few laboratories which have more sensible equipments, being more expensive. Having in mind this problem, the present work aims the development of methods that are simple, fast, cheap, repeatable and cleaner using diffuse reflectance spectroscopy. The developed methods consists in the reaction of furosemide with the chromogenic reagent iron(III) chloride (FeCl3) in a micellar medium of dodecyltrimethylammonium bromide (DTAB) and in the reaction of lead ion (Pb2+) with sodium rhodizonate (ROD) in a micellar medium of sodium dodecyl sulfate (SDS), which concentrations were optimized by chemometrics. The reactions were realized as spot test using Whatman qualitative filter paper as a solid support, involving the formation of a colored product in 477 nm for furosemide and 545 nm for lead ion. The analytical curves were constructed from standard solutions of furosemide and lead. The Limit of Detection (LoD) and the Limit of Quantification (LoQ) were, respectively, 0,49 and 1,62 mmol L-1 for furosemide and 1,12 and 3,75 ppm for lead, accordingly to the recommendations of IUPAC. The proposed methods were applied for the determination of furosemide in synthetic and human urine and for the determination of lead in gunshot residues (GSRs) and in commercial sugar cane brandy, with the... (Complete abstract click electronic access below)
Descrição
Palavras-chave
Quimica analitica, Química legal
Como citar
LUIZ, Vitor Hugo Marques. Desenvolvimento de métodos analíticos limpos para determinações forenses: chumbo em resíduos de disparo e furosemida em doping. 2012. 113 f. Dissertação (mestrado) - Universidade Estadual Paulista, Instituto de Química, 2012.