Department of Analytical Chemistry, Faculty of Chemistry, Universidad Complutense de Madrid, Ciudad Universitaria s/n, E-28040 Madrid, Spain.
Anal Chem. 2011 Mar 15;83(6):2046-55. doi: 10.1021/ac102839n. Epub 2011 Feb 21.
The present work describes the development of a sensitive and highly selective innovative method for the simultaneous detection of six fluoroquinolone (FQ) antimicrobials (enrofloxacin, ciprofloxacin, norfloxacin, levofloxacin, danofloxacin, and sarafloxacin) in water samples. This detection is based on online solid phase extraction, coupled to liquid chromatography (LC), using for the first time tailor-made molecularly imprinted microspherical polymer particles prepared via precipitation polymerization. Various parameters affecting the extraction efficiency of the polymer have been optimized to reduce nonspecific interactions and to achieve selective uptake of the antibiotics from real samples. The method shows good recoveries ranging between 62% and 102% (V = 25 mL) for the different FQs tested and excellent interday and intraday precision with relative standard deviation (RSD) values between 2-5% and 2-6%, respectively. The detection limits were between 1-11 ng L(-1) (drinking water) and 1-12 ng L(-1) (fish farm water) when 25 mL samples were processed. The polymer showed selectivity for FQs containing a piperazine moiety whereas no retention was found for other antibiotics or nonrelated compounds. The method has been applied to the analysis of trace amounts of the FQs tested in drinking and fish farm water samples with excellent recoveries (>91%) and good precision (RSDs <5%).
本工作开发了一种灵敏且高度选择性的创新方法，用于同时检测水样中的六种氟喹诺酮（FQ）抗菌药物（恩诺沙星、环丙沙星、诺氟沙星、左氧氟沙星、丹诺沙星和沙拉沙星）。该检测基于在线固相萃取，与液相色谱（LC）联用，首次使用通过沉淀聚合制备的定制分子印迹微球聚合物颗粒。优化了各种影响聚合物萃取效率的参数，以减少非特异性相互作用，并从实际样品中实现抗生素的选择性摄取。该方法对不同 FQ 的回收率在 62%-102%之间（V = 25 mL），具有良好的日间和日内精密度，相对标准偏差（RSD）值分别在 2%-5%和 2%-6%之间。当处理 25 mL 样品时，检测限在 1-11 ng L(-1)（饮用水）和 1-12 ng L(-1)（养鱼场水）之间。该聚合物对含有哌嗪部分的 FQ 具有选择性，而对其他抗生素或非相关化合物没有保留。该方法已应用于饮用水和养鱼场水样中痕量 FQ 的分析，回收率>91%，精密度良好（RSDs <5%）。
