Department of Analytical Chemistry, Faculty of Chemistry, University of Seville, Seville, Spain.
Anal Bioanal Chem. 2013 Mar;405(8):2575-84. doi: 10.1007/s00216-012-6664-5. Epub 2013 Jan 11.
For the first time, an electromembrane extraction combined with a HPLC procedure using diode array and fluorescence detection has been developed for the determination of seven widely used fluoroquinolones (FQs): marbofloxacin, norfloxacin, ciprofloxacin, danofloxacin, enrofloxacin, gatifloxacin and grepafloxacin. The drugs were extracted from acid aqueous sample solutions (pH 5), through a supported liquid membrane consisting of 1-octanol impregnated in the walls of a S6/2 Accurel® polypropylene hollow fiber, to an acid (pH 2) aqueous acceptor solution inside the lumen of the hollow fiber. The main operational parameters were optimized, and extractions were carried out in 15 min using a potential of 50 V. Enrichment factors of 40-85 have been obtained using only 15 min of extraction time versus 330 min used in a previously proposed hollow-fiber liquid-phase microextraction procedure. The procedure allows low detection and quantitation limits of 0.005-0.07 and 0.007-0.15 μg L(-1), respectively. The proposed method was successfully applied to the FQs analysis in urban wastewaters.
首次开发了一种电膜萃取-高效液相色谱法，结合二极管阵列和荧光检测，用于测定七种广泛使用的氟喹诺酮类药物（FQs）：马波沙星、诺氟沙星、环丙沙星、丹诺沙星、恩诺沙星、加替沙星和 grepafloxacin。这些药物从酸性水性样品溶液（pH 5）中提取，通过 1-辛醇浸渍在 S6/2 Accurel® 聚丙烯中空纤维壁中的支撑液膜，进入中空纤维内腔中的酸性（pH 2）水性接受溶液中。优化了主要操作参数，并在 50 V 的电位下 15 分钟内进行了萃取。与先前提出的中空纤维液相微萃取程序中使用的 330 分钟相比，仅使用 15 分钟的萃取时间即可获得 40-85 的富集因子。该程序允许检测和定量限分别为 0.005-0.07 和 0.007-0.15 μg L(-1)。该方法成功应用于城市废水中 FQs 的分析。
