On-line anion exchange solid-phase extraction coupled to liquid chromatography with fluorescence detection to determine quinolones in water and human urine

• Published in: Journal of Chromatography A 2013-10, Vol.1310, p.91-97
• Main Authors: Lara, Francisco J., del Olmo-Iruela, Monsalud, García-Campaña, Ana M.
• Format: Article
• Language: English
• Subjects: Analysis; Analytical chemistry; anion exchange; Anion exchanging; Applied sciences; Biological and medical sciences; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography; detection limit; Drinking water and swimming-pool water. Desalination; Exact sciences and technology; Extraction; Fluorescence; General pharmacology; Human; humans; Liquid chromatography; Medical sciences; On-line solid-phase extraction; Other chromatographic methods; Pharmacology. Drug treatments; Pollution; pumps; Quinolones; solid phase extraction; Tap water; Urine; Water; Water treatment and pollution
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2013.08.071

•On-line SPE coupled to LC with fluorescence detection to monitoring quinolones.•The anion exchange sorbent for SPE makes highly compatible the on-line coupling with LC.•Determination of 11 quinolones directly in waters with LOD between 7 and 110ng/L.•Determination of 9 quinolones in diluted urine with recoveries between 93.6 and 108.6%. An analytical method based on on-line solid-phase extraction coupled to liquid chromatography with fluorescence detection has been developed to determine quinolones in tap water and human urine. A home-made setup was used to percolate 10mL of sample through a solid-phase extraction column. Analytes were retained onto the sorbent by an anion exchange mechanism which ensures an optimum compatibility with the subsequent chromatographic separation. A C-18 column containing core-shell particles (2.6μm) was used to achieve peak efficiencies up to 200,000plates/m, at a flow rate of 1.2mL/min and without the need for special pumps. The method allowed the determination of 11 quinolones directly in tap water samples in less than 20min and with limits of detection ranging between 7 and 110ng/L. The sensitivity achieved made possible the direct determination of 9 quinolones in human urine without any sample treatment, just dilution with water. Relative recoveries between 94 and 109% were obtained meaning that the matrix effect in human urine is negligible after dilution. Satisfactory results were also obtained in terms of precision since relative standard deviations were always below 13%.