Separation of fifteen quinolones by high performance liquid chromatography: application to pharmaceuticals and ofloxacin determination in urine.
A simple chromatographic method is described for assaying 15 quinolones and fluoroquinolones (pipemidic acid, marbofloxacin, enoxacin, ofloxacin, norfloxacin, ciprofloxacin, danofloxacin, lomefloxacin, enrofloxacin, sarafloxacin, difloxacin, oxolinic acid, nalidixic acid, flumequine and piromidic acid), in urine and pharmaceutical samples. The determination was achieved by LC using an RP C18 analytical column. A mobile phase composed of mixtures of methanol-ACN-10 mM citrate buffer at pH 3.5 and 10 mM citrate buffer at pH 4.5, delivered under an optimum gradient program, at a flow rate of 1.5 mL/min, allows to accomplish the chromatographic separation in 26 min. For detection, diode-array UV-Vis at 280 nm and fluorescence detection set at excitation wavelength/emission wavelength: 280/450, 280/ 495, 280/405 and 320/360 nm were used. Detection and quantification limits were between 0.3-18 and 0.8-61 ng/mL, respectively. The method was validated in terms of interday (n = 6) and intraday (n = 6) precision and accuracy. The procedure was successfully applied to the analysis of human and veterinary pharmaceuticals. Also, ofloxacin was determined in human urine samples belonging to a patient undergoing treatment with this active principle, among others.
Cañada-Cañada
Florentina
F
Department of Analytical, Chemistry, University of Extremadura, 06071 Badajoz, Spain. flori@unex.es
Espinosa-Mansilla
Anunciación
A
Muñoz de la Peña
Arsenio
A
D000818:Animals; D002851:Chromatography, High Pressure Liquid; D006801:Humans; D015242:Ofloxacin / Q000652:urine*; D004364:Pharmaceutical Preparations / Q000032:analysis* / Q000652:urine; D015363:Quinolones / Q000032:analysis* / Q000302:isolation & purification* / Q000652:urine
D004364:Pharmaceutical Preparations; D015363:Quinolones; D015242:Ofloxacin