Determination of the chemotherapeutic quinolonic and cinolonic derivatives in urine by high-performance liquid chromatography with ultraviolet and fluorescence detection in series.
An HPLC method with ultraviolet and fluorimetric detection has been established for the separation and determination of six quinolonic and cinolonic antibiotics. A Nova-Pak C18 column (150 x 3.9 mm) and a Waters 486 UV and a Waters 470 fluorescence detector have been used. The influence of variables such as mobile-phase composition and flow-rate, has been studied. An acetonitrile-aqueous solution of oxalic acid 4x10(-4) M (28:72, v/v) has been selected as optimum. The wavelength for the photometric detection of the six antibiotics was 265 nm. For the fluorimetric detection two pairs of excitation/emission wavelengths, 260/360 or 270/440 nm, were selected for the determination of nalidixic acid, 7-hydroxymethylnalidixic acid and oxolinic acid, and for the determination of pipemidic acid and cinoxacin, respectively. The analytical parameters and detection and quantification limits of the method have been determined. The proposed method has been applied for the determination of the six compounds in urine, applying different procedures depending on their concentration, the results being very acceptable.
Durán Merás
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Department of Analytical Chemistry, Faculty of Sciences, University of Extremadura, Badajos, Spain.
Galeano Díaz
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Rodriguez Cáceres
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Salinas López
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D000890:Anti-Infective Agents / Q000652:urine*; D002851:Chromatography, High Pressure Liquid; D002937:Cinoxacin / Q000652:urine; D006801:Humans; D009268:Nalidixic Acid / Q000652:urine; D010093:Oxolinic Acid / Q000652:urine; D010876:Pipemidic Acid / Q000652:urine; D010893:Piromidic Acid / Q000652:urine; D012680:Sensitivity and Specificity; D013050:Spectrometry, Fluorescence; D013056:Spectrophotometry, Ultraviolet
D000890:Anti-Infective Agents; D009268:Nalidixic Acid; D010893:Piromidic Acid; D010093:Oxolinic Acid; D002937:Cinoxacin; D010876:Pipemidic Acid