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Previous issue date: 2015-02-06 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior (CAPES) / Guanilhidrazonas s?o uma classe de subst?ncias amplamente estudadas por apresentar grande potencial biol?gico. A an?lise de f?rmacos e medicamentos ? ferramenta importante para garantir qualidade, seguran?a e efic?cia aos novos medicamentos. Nesse estudo foram avaliadas as guanilhidrazonas sint?ticas WE005 (3,4-dimetoxibenzalde?doguanilhidrazona), WE015 (benzalde?doguanilhidrazona) e WE016 (metil-4-formilbenzoatoguanilhidrazona) com o objetivo de caracterizar, desenvolver e validar m?todo anal?tico utilizando t?cnicas t?rmicas (DSC e TG), espectrosc?pica (FTIR), microsc?pica (MEV) e cromatogr?fica (CLUE/DAD). Na caracteriza??o por DSC e TG foram utilizadas as seguintes raz?es de aquecimento: 2,5; 5,0; 10 e 20 ?C/min em atmosfera de nitrog?nio (50 mL/min) at? 500?C (DSC) e 900?C (TG). A an?lise na regi?o do infravermelho m?dio das mol?culas foi realizada a temperatura ambiente e na faixa de fus?o. Os espectros foram comparados atrav?s da correla??o de Pearson utilizando o algoritmo ad hoc. O estudo cin?tico foi feito atrav?s do m?todo de Ozawa. O planejamento fatorial investigou a influ?ncia do comprimento da coluna, fluxo e propor??o de fase m?vel sobre o tempo de reten??o, fator de cauda, resolu??o e n?mero de pratos te?ricos. As t?cnicas t?rmicas foram capazes de caracterizar as mol?culas atrav?s de suas transi??es de fase e etapas na curva termogravim?trica, informando ainda sobre a estabilidade t?rmica, com temperatura inicial de decomposi??o em torno de 240 ?C. O estudo cin?tico mostrou que todas as mol?culas apresentam ordem zero e que a amostra WE016 apresentou maior energia de ativa??o. Os espectros de infravermelho de acordo com a correla??o de Pearson apresentaram mudan?as significativas entre a temperatura ambiente e o espectro da faixa de fus?o. O planejamento fatorial atrav?s dos gr?ficos de superf?cie-resposta e Pareto revelou que a vari?vel de maior influ?ncia sobre todas as vari?veis dependentes foi o comprimento da coluna. O melhor m?todo para a separa??o das guanilhidrazonas deste estudo foi: coluna C18 (50 mm x 2 mm t.p. 2.2 ?m), fase m?vel MeOH:H2O:TEA 40:60:0,1, pH 3,5 ajustado com ?cido ac?tico; fluxo de 0,2 mL/min, temperatura do forno 30 ?C. A concentra??o final das guanilhidrazonas foi de 30 ?g/mL e foram detectadas simultaneamente atrav?s do comprimento de onda de 290 nm. Um m?todo r?pido foi desenvolvido para separar as guanilhidrazonas WE005, WE015 E WE016 por CLUE/DAD. Planejamento fatorial foi uma ferramenta ?til para o desenvolvimento racional do m?todo. / Guanilhidrazonas substances are widely studied for presenting great biological potential, especially antitumor activity, antimicrobial, antimalarial, antifungal and anti-hypertensive. This study assessed the synthetic guanylhydrazones WE005 ((2-[(3,4-dimethoxyphenyl)methylene]-hydrazinecarboximidamide),WE015 (2(phenylmethylene)-hydrazinecarboximidamide) and WE016 (4-[[2-(aminoiminomethyl) hydrazinylidene]methyl]-benzoic acid methyl ester) in order to characterize and develop analytical method using thermal techniques (DSC and TGA), spectroscopic (FTIR ) and microscopic (SEM) and chromatographic (UHPLC / DAD). The characterization by DSC and TG were used the following heating rates: 2.5; 5.0; 10 and 20 ? C / min in a nitrogen atmosphere (50 ml / min) to 500 ? C (DSC) and 900 ? C (TG). The kinetic study was done by Ozawa method. The analysis in the mid-infrared region of molecules was performed at room temperature and the melting temperature. The spectra were compared using Pearson's correlation using ad hoc algorithm. For the development of the analytical method was used factorial design. Thermal techniques have been able to characterize the molecules through their phase transitions and steps in the thermogravimetric curve, and telling about the thermal stability, with an initial decomposition temperature of about 240 ? C. The kinetic study showed that the speed of the thermal decomposition of molecules has zero order and that the WE016 sample showed higher activation energy. Infrared spectra according to the Pearson correlation showed significant changes between the room temperature and the melting range of the spectrum. The factorial design through surface-response graphs and Pareto showed that the most influential variable on all dependent variables was the length of the column. The best method for the separation of guanylhydrazones this study was: C18 column (50 mm x 2 mm tp 2.2 microns), mobile phase MeOH: H2 O: TEA 40: 60: 0.1, pH 3.5 adjusted with acetic acid; flow rate of 0.2 ml / min, oven temperature 30 ? C. The final concentration of guanylhydrazones was 30 mg / mL and were detected simultaneously by a wavelength of 290 nm. A rapid method was developed to separate guanylhydrazones WE005, WE015 and WE016 by CLUE / DAD. Factorial design was a useful tool for the rational development of the method.
| Identifer | oai:union.ndltd.org:IBICT/oai:repositorio.ufrn.br:123456789/21493 |
| Date | 06 February 2015 |
| Creators | Dantas, Monique Gomes |
| Contributors | 02820912460, Souza, F?bio Santos de, 92771300400, Moura, Maria de F?tima Vit?ria de, 31482015404, Arag?o, Cicero Fl?vio Soares, Gomes, Ana Paula Barreto |
| Publisher | PROGRAMA DE P?S-GRADUA??O EM CI?NCIAS FARMACEUTICAS, UFRN, Brasil |
| Source Sets | IBICT Brazilian ETDs |
| Language | Portuguese |
| Detected Language | English |
| Type | info:eu-repo/semantics/publishedVersion, info:eu-repo/semantics/masterThesis |
| Source | reponame:Repositório Institucional da UFRN, instname:Universidade Federal do Rio Grande do Norte, instacron:UFRN |
| Rights | info:eu-repo/semantics/openAccess |
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