RESUMEN
A simple and sensitive high performance liquid chromatography with fluorescence detection (HPLC–FD) has been developed for simultaneous quantification of doxorubicin (DOX) and its dipeptide conjugate prodrug (PDOX) in mice plasma. The chromatographic separation was carried out on an Amethyst C18–H column with gradient mobile phase of 0.1%formic acid and 0.1%formic acid in acetonitrile at a flow rate of 1.0 mL/min. The excitation and emission wavelengths were set at 490 and 550 nm, respectively. The method was comprehensively validated. The limits of detection were low up to 5.0 ng/mL for DOX and 25.0 ng/mL for PDOX. And the limits of quantification were low up to 12.5 ng/mL for DOX and 50 ng/mL for PDOX, which were lower than those for most of the current methods. The calibration curves showed good linearity (R2 4 0.999) over the concentration ranges. The extraction recoveries ranged from 84.0%to 88.2% for DOX and from 85.4% to 89.2% for PDOX. Satisfactory intra-day and inter-day precisions were achieved with RSDs less than 9.1%. The results show that the developed HPLC–FD method is accurate, reliable and will be helpful for preclinical pharmacokinetic study of DOX and PDOX.
RESUMEN
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.