DESENVOLVIMENTO DE METODOLOGIA ANALÍTICA PARA QUANTIFICAÇAO DE FÁRMACOS EM MEIO AQUÁTICO POR EXTRAÇAO EM FASE SÓLIDA E HPLC.
DOI:
https://doi.org/10.18316/167Keywords:
fármacos, SPE, HPLC-UVAbstract
O presente trabalho apresenta o desenvolvimento de uma metodologia analítica para fármacos em nível de traços como poluentes no meio aquoso, envolvendo o uso de cromatografia líquida com detector espectrofotométrico na região do ultravioleta (HPLC-UV). Quatro fármacos (antibióticos), a saber: ampicilina, amoxilina, tetraciclina e cefalexina, foram avaliados em presença de diversas fases móveis, que foram selecionadas de acordo com a melhor performance cromatográfica, sendo que ampicilina e amoxilina apresentaram melhor performance cromatográfica na mesma fase móvel. Para extração em fase sólida dos fármacos foram avaliadas três fases comerciais: LC-18 (SUPELCLEAN), Supelclean TM ENVI TM-Chrom P, Abselut NEXUS. Amoxilina e ampicilina não apresentaram boas recuperações nas fases e eluentes estudados. Para tetraciclina e cefalexina, a fase comercial Chrom P apresentou boas recuperações quando utilizados os solventes metanol e a mistura 1% de solução aquosa de ácido acético e metanol (60:40), respectivamente.
Palavras-chave: fármacos; SPE; HPLC-UV.
ABSTRACT
Development of analytical methodology for quantification of pharmaceuticals in aqueos milieu by solid phase extraction and high performance liquid chromatography. The present work propose the development of an analytical methodology for pharmaceuticals at trace levels in aqueous milieu, combining the use of solid phase extraction and high performance liquid chromatography, employing UV-vis detector (HPLC-UV). Four pharmaceuticals (antibiotics), namely: ampicillin, amoxilin, tetraciclin and cephalexin, were evaluated in the presence of different mobile phases, which were selected according to the best performance. Ampicilin and amoxilin showed the best performance in the same mobile phase. For the solid phase extraction procedure, three commercial phases were evaluated: LC-18 (SUPELCLEAN), Supelclean TM ENVITM-Chrom P and Abselut NEXUS. Amoxilin and amphcillin did not show good recovey in the evaluated phases and eluents. For tetraciclin and cephalexin, the commercial phase Chrom P showed the best performance using methanol as solvent and a 1% acetic acid/methanol (60:40) mixture.
Key words: pharmaceuticals, SPE, HPLC-UV
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