Departamento de Medio Ambiente, INIA, Carretera de A Coruña km 7.5, 28240 Madrid, Spain.
Departamento de Medio Ambiente, INIA, Carretera de A Coruña km 7.5, 28240 Madrid, Spain.
J Chromatogr A. 2014 Aug 29;1357:158-64. doi: 10.1016/j.chroma.2014.04.038. Epub 2014 Apr 18.
In this work, molecularly imprinted polymer (MIP) beads have been prepared and evaluated for the development of a supported liquid membrane-protected micro-solid phase extraction method for the analysis of sulfonamides (SAs) in aqueous samples. The performance of MIP beads was firstly evaluated in cartridges by conventional solid-phase extraction for the simultaneous analysis of SAs. Afterward, beads were packed into a polypropylene hollow fiber protected by an organic solvent immobilized in the pores of the capillary wall. During the process, the analytes were extracted from the aqueous sample to the immobilized organic solvent and then selectively retained by the MIP beads located inside the capillary. The effect of various experimental parameters as sample pH, time and stirring-rate among others, were studied for the establishment of optimum rebinding conditions. Relative recoveries for all sulfonamides tested in river and reservoir water samples by the proposed method using 100mL water sample spiked with 50μg L-1 of each sulfonamide were within 70-120%, with a relative standard deviation (RSD) <10% (n=3). The detection limits (LODs) were within 0.2-3μgL(-1), depending upon the sulfonamide and the type of water used.
在这项工作中,制备了分子印迹聚合物(MIP)珠,并对其进行了评估,以开发用于分析水样中磺胺类药物(SAs)的支持液膜保护微固相萃取方法。首先通过常规固相萃取在小柱中评估 MIP 珠对磺胺类药物的同时分析性能。然后,将珠装入由固定在毛细管壁孔中的有机溶剂保护的聚丙烯中空纤维中。在此过程中,将分析物从水样中萃取到固定的有机溶剂中,然后由位于毛细管内的 MIP 珠选择性保留。研究了各种实验参数,例如样品 pH 值、时间和搅拌速率等,以确定最佳的结合条件。使用 100mL 水样,在河水和水库水样中加入 50μg L-1 的每种磺胺类药物,用所提出的方法对所有磺胺类药物进行测试,相对回收率在 70-120%之间,相对标准偏差(RSD)<10%(n=3)。检测限(LODs)在 0.2-3μg L-1 之间,具体取决于所用的磺胺类药物和水样的类型。