Department of Analytical Chemistry, University of Granada, Campus Fuentenueva S/N, E-18071 Granada, Spain.
J Chromatogr A. 2013 Oct 4;1310:91-7. doi: 10.1016/j.chroma.2013.08.071. Epub 2013 Aug 23.
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 10 mL 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 (2.6 μm) was used to achieve peak efficiencies up to 200,000 plates/m, at a flow rate of 1.2 mL/min and without the need for special pumps. The method allowed the determination of 11 quinolones directly in tap water samples in less than 20 min and with limits of detection ranging between 7 and 110 ng/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%.
建立了一种基于在线固相萃取-液相色谱-荧光检测法的分析方法，用于测定自来水中和人尿中的喹诺酮类药物。采用自制装置通过固相萃取柱渗滤 10 mL 样品。分析物通过阴离子交换机制保留在吸附剂上，这确保了与后续色谱分离的最佳兼容性。使用含有核壳颗粒（2.6 μm）的 C-18 柱，在流速为 1.2 mL/min 时达到了高达 200,000 板/m 的峰效率，而无需特殊的泵。该方法允许在不到 20 分钟的时间内直接测定自来水中的 11 种喹诺酮类药物，检测限范围在 7 至 110 ng/L 之间。所达到的灵敏度使得可以直接在未经任何样品处理的情况下，仅用水稀释，就可以测定人尿中的 9 种喹诺酮类药物。通过稀释，人尿中的基质效应可忽略不计，获得了 94%至 109%的相对回收率。在精密度方面也取得了令人满意的结果，因为相对标准偏差始终低于 13%。
