Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran, Iran.
J Pharm Biomed Anal. 2012 Jul;66:264-70. doi: 10.1016/j.jpba.2012.03.028. Epub 2012 Mar 24.
A simple microextraction method based on emulsification of organic extraction solvent in aqueous sample using an ionic surfactant was evaluated for extraction and preconcentration of trace amounts of ofloxacin and ciprofloxacin as polar model drugs. In this method, the surfactant was used as carrier and disperser agent simultaneously. The target analytes were converted into their ion-pair complexes with Aliquat-336 and then extracted into an organic solvent (1-octanol) dispersed in aqueous solution. After extraction and phase separation, the organic solvent on top of the solution was withdrawn into the syringe and 20 μL of it was injected into a HPLC instrument for analysis. The factors influential to extraction were investigated and optimized. Under optimum extraction conditions, the limits of detection (LODs) as small as 0.06 and 0.02 ng mL(-1) and linear dynamic range of 0.1-100 and 0.06-100 ng mL(-1) were obtained for ofloxacin and ciprofloxacin, respectively. For analysis of real samples such as waste water, river water and urine samples, solid-phase extraction (SPE) was applied prior to liquid phase microextraction in order to avoid/remove matrix effect. The obtained results indicate that the proposed method is efficient, fast and inexpensive for extraction and determination of fluoroquinolones in environmental aqueous and urine samples.
一种简单的基于离子型表面活性剂增敏的有机溶剂微萃取方法被用于痕量氧氟沙星和环丙沙星的萃取和预富集。在该方法中,表面活性剂同时作为载体和分散剂。目标分析物被转化为与 Aliquat-336 的离子对配合物,然后萃取到分散在水溶液中的有机溶剂(1-辛醇)中。萃取和相分离后,将溶液顶部的有机溶剂用注射器吸入,并取 20 μL 注入 HPLC 仪器进行分析。考察并优化了影响萃取的因素。在最佳萃取条件下,氧氟沙星和环丙沙星的检测限(LOD)分别低至 0.06 和 0.02 ng mL(-1),线性动态范围分别为 0.1-100 和 0.06-100 ng mL(-1)。对于废水、河水和尿液等实际样品的分析,在液相微萃取之前应用固相萃取(SPE)以避免/去除基质效应。结果表明,该方法对于环境水样和尿液中氟喹诺酮类药物的提取和测定是高效、快速且廉价的。