Estudo da derivatiza??o de glyphosate e AMPA utilizando FMOC-CL e BSTFA para an?lises cromatogr?ficas

• Main Author: Catrinck, Tereza Cristina Pimenta Gon?alves
• Other Authors: Mozzer, Otto Domenici
• Language: Portuguese
• Published: UFVJM 2014
• Subjects: ?cido aminometilfosf?nico; Derivatiza??o; Glyphosate
• Online Access: http://acervo.ufvjm.edu.br:8080/jspui/handle/1/295

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No. of bitstreams: 2 tereza_cristina_pimenta_goncalves_catrinck.pdf: 1238472 bytes, checksum: 651b04064f25bbcb2260de4d863373f2 (MD5) license_rdf: 23898 bytes, checksum: e363e809996cf46ada20da1accfcd9c7 (MD5) Previous issue date: 2013 === Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior (Capes) === Com este trabalho, objetivou-se otimizar simultaneamente metodologias para derivatiza??o de glyphosate (GLY) e ?cido aminometilfosf?nico (AMPA) para an?lises por cromatografia gasosa acoplada a espectrometria de massas (CG-EM) e cromatografia l?quida de alta efici?ncia com detector ultravioleta (CLAE-UV). Al?m disso, foram otimizadas as condi??es cromatogr?ficas por CLAE-UV para a an?lise destes compostos. O GLY foi selecionado para o estudo por ser um herbicida amplamente utilizado para o controle de pragas que, junto ao seu principal metab?lito secund?rio (AMPA) apresenta potencial risco toxicol?gico para a sa?de humana e para o meio ambiente. Devido aos seus efeitos delet?rios, alguns m?todos anal?ticos t?m sido desenvolvidos a fim de monitorar seus res?duos no meio ambiente. M?todos cromatogr?ficos t?m sido preferencialmente usados, contudo as mol?culas em estudo apresentam baixa volatilidade e aus?ncia de grupos crom?foros, sendo necess?rio adicionar etapas de derivatiza??o. Neste trabalho foram avaliadas duas metodologias para derivatiza??o das mol?culas de GLY e AMPA: com piririna e N-O(bistrimetilsilil)trifluoroacetamida (BSTFA) para an?lises por CG-EM e com cloroformiato de 9-fluorenilmetila (FMOC-Cl) para an?lises por CLAE-UV. A utiliza??o de piridina:BSTFA em propor??o 60:100, respectivamente, sem vibra??o ultrass?nica e ajuste de pH resultaram em condi??es ?timas de an?lises por CG-EM. J? para an?lises por CLAE-UV, tamp?o borato 200 mmol L-1, FMOC-Cl 500 mg L-1, homogeneiza??o por 5 minutos, an?lise imediatamente ap?s a rea??o e lavagem com ?ter diet?lico promoveram resultados satisfat?rios. Finalmente, as condi??es ?timas de an?lise por CLAE-UV foram estudas e determinou-se que a fase m?vel composta por acetonitrila/tamp?o fosfato, comprimento de onda 260 nm, gradiente com propor??o de 25:75 v/v (0-2,5 minutos), 65:35 v/v (4,5-10 minutos) e 25:75 v/v (11-12 minutos) apresentaram melhores resultados. === Disserta??o (Mestrado) ? Programa de P?s-Gradua??o em Qu?mica, Universidade Federal dos Vales do Jequitinhonha e Mucuri, 2013. === ABSTRACT This study aimed to optimize both methodologies for derivatization of glyphosate (GLY) and aminomethylphosphonic acid (AMPA) for analysis by gas chromatography-mass spectrometry (GC-MS) and high performance liquid chromatography with ultraviolet detector (HPLC-UV). Moreover, the chromatographic conditions were optimized by HPLC-UV for the analysis of these compounds. The GLY was selected for the study because it is a herbicide widely used for pest control that, with its main secondary metabolite (AMPA) has potential toxicological risk to human health and the environment. Due to the deleterious effects, some analytical methods have been developed to monitor their residues on the environment. Chromatographic methods have been used preferentially, however the molecules in study have low volatility and absence of chromophoric groups being necessary to add derivatization steps. In this work were evaluated two methodologies for derivatization of GLY and AMPA molecules: pyridine and N-O(bistrimethylsilyl)trifluoroacetamide (BSTFA) for analysis by GC-MS and 9-fluorenylmethyl chloroformate (FMOC-Cl) for analysis by HPLC-UV. The use of pyridine:BSTFA in ratio 60:100, respectively, without ultrasonic vibration and adjustment pH result in better analyses conditions by GC-MS. Already for analysis by HPLC-UV, borate buffer 200 mmol L-1, FMOC-Cl 500 mg L-1, homogenization for 5 minutes, analysis immediately after reaction and washing with diethyl ether promoted satisfactory results. Finally, the optimal conditions for analysis by HPLC-UV were studied and it was determined that the mobile phase consisting of acetonitrile / phosphate buffer, wavelength 260 nm, ratio gradient 25:75 v / v (0-2.5 minutes ), 65:35 v / v (4.5-10 minutes), 25:75 v / v (11-12 minutes) showed better results.