RESUMEN
Pharmaceuticals are emerging contaminants and it must be noted that approximately 70 % of them are excreted via urine. Therefore, urine usage implies the risk of transfer of pharmaceutical residues to agricultural fields and environment contamination. Thus, this study aimed on the development and validation of a LC-MS/MS method for D-norgestrel (D-NOR) and progesterone (PRO) determination in human urine, as well as the evaluation of the removal efficiency of two methods (storage and evaporation), and the effects of acidification with sulfuric acid. The storage process was evaluated for 6 weeks, while the evaporation was assessed at three different temperatures (50, 75, and 100 °C). All experiments were done with normal urine (pH = 6.0) and acidified urine (pH = 2.0, with sulfuric acid). The results of validation showed good method efficiency. In the second week of storage, higher hormone degradation was observed. In the evaporation method, both D-NOR and PRO were almost completely degraded when the volume was reduced to the lowermost level. Results also indicate that acidification did not affect degradation. Overall, the results showed that combination of two methods can be employed for more efficient hormone removal in urine.
Asunto(s)
Monitoreo del Ambiente/métodos , Levonorgestrel/aislamiento & purificación , Progesterona/aislamiento & purificación , Orina/química , Adulto , Cromatografía Liquida , Voluntarios Sanos , Humanos , Levonorgestrel/orina , Límite de Detección , Masculino , Progesterona/orina , Reproducibilidad de los Resultados , Manejo de Especímenes , Espectrometría de Masas en Tándem/métodos , Temperatura , Volatilización , Adulto JovenRESUMEN
Processos de tratamentos têm sido alvo de estudos com a finalidade de promover a remoção dos fármacos na urina humana de forma a garantir a segurança ambiental da utilização dessa como fertilizante na agricultura. Neste artigo foi desenvolvido e validado um método de CLAE-DF para a determinação simultânea de ofloxacina, norfloxacina e ciprofloxacina na urina humana. O método proposto descreve uma alternativa eficaz para a determinação de resíduos de fluoroquinolonas, eliminando o passo de limpeza. Além disso, o método proposto demonstrou ser seletivo, com boa linearidade (r>0,99), sensibilidade, precisão (80% a 107%) e repetitividade. Este método mostra ser adequado para análises de rotina (de baixo custo, simples, e utilizando pequeno volume de solventes) para abordagens ecológicas.
Treatment processes have been the focus of studies aiming at promoting the removal of drugs in human urine in order to ensure environmental safety using it as a fertilizer in agriculture. So, an HPLC-FD method for the simultaneous determination of ofloxacin, norfloxacin and ciprofloxacin in human urine was developed and validated. The proposed method describes an efficient alternative for the determination of fluoroquinolone residues by eliminating the clean-up step. Moreover, the proposed method proved to be selective, with good linearity (r>0.99), sensitivity, accuracy (80% to 107%) and repeatability. This method shows to be suitable for routine analyses (simple, low price and using a small volume of solvents) for ecological approaches.