Czyz Ewelina, Erben Jakub, Vinter Jan, Švec František, Šatínský Dalibor
Charles University, Faculty of Pharmacy in Hradec Králové, Department of Analytical Chemistry, Ak. Heyrovského 1203, 500 05, Hradec Králové, Czech Republic.
The Technical University of Liberec, Faculty of Textile Engineering, Department of Nonwovens and Nanofibrous Materials, Studentská 1402/2, 46001, Liberec 1, Czech Republic.
Anal Chim Acta. 2024 Oct 23;1327:343137. doi: 10.1016/j.aca.2024.343137. Epub 2024 Aug 22.
A novel supported liquid extraction approach using small polymeric nanofibrous discs was demonstrated and applied to the analysis of real river water. Nanofibrous discs were tested to extract model mixture of 9 common water contaminants 4-nitrophenol, various chlorophenols, bisphenol A, permethrin, and fenoxycarb featuring a wide range of log P values (1.9-6.5). Polyacrylonitrile, polyhydroxybutyrate, and polylactic acid nanofibers were selected as adsorptive materials. One-step desorption was performed directly in HPLC vials, to avoid time-consuming evaporation and reconstitution steps. The discs were allowed to sediment to the bottom of the vial before injection into the chromatographic system.
Various parameters affecting the extraction efficiency including 1-octanol volume, extraction time, ionic strength, and sample volume were investigated and optimized. Wetting the nanofiber discs with 1-octanol resulted in up to 20-fold increase in enrichment factor when compared to non-wetted polymer counterparts. The highest enrichment factors were observed for analytes with a log P range of 3.3-4.5. Our developed method showed good linearity in the range 20-200 μg/L for all analytes tested. Satisfactory repeatability with RSD <13 % were achieved covering all steps including disc preparation, wetting, extraction/elution, and chromatography analysis, and recoveries ranged from 58.93 to 121.43 %.
This work represents novel simple supported liquid extraction approach using impregnated polymer nanofiber discs. Using only 50 μL 1-octanol, we reduced the organic solvent compared to other extraction methods. There was no need for any plastic cartridge to hold the sorbent and direct in-vial desorption reduced the unnecessary, time-consuming steps and simplified the sample preparation protocol.
展示了一种使用小型聚合物纳米纤维盘的新型支撑液液萃取方法，并将其应用于实际河水的分析。对纳米纤维盘进行了测试，以萃取9种常见水中污染物的模型混合物，包括4-硝基苯酚、各种氯酚、双酚A、氯菊酯和苯氧威，这些污染物的log P值范围很广（1.9 - 6.5）。选择聚丙烯腈、聚羟基丁酸酯和聚乳酸纳米纤维作为吸附材料。直接在HPLC小瓶中进行一步解吸，以避免耗时的蒸发和重构步骤。在注入色谱系统之前，让盘沉淀到小瓶底部。
研究并优化了影响萃取效率的各种参数，包括正辛醇体积、萃取时间、离子强度和样品体积。与未湿润的聚合物对应物相比，用正辛醇湿润纳米纤维盘可使富集因子提高多达20倍。对于log P范围为3.3 - 4.5的分析物，观察到最高的富集因子。我们开发的方法对所有测试分析物在20 - 200μg/L范围内显示出良好的线性。包括盘制备、湿润、萃取/洗脱和色谱分析在内的所有步骤都实现了令人满意的重复性，相对标准偏差（RSD）<13%，回收率范围为58.93%至121.43%。
这项工作代表了一种使用浸渍聚合物纳米纤维盘的新型简单支撑液液萃取方法。与其他萃取方法相比，仅使用50μL正辛醇，我们减少了有机溶剂的使用。无需任何塑料柱来容纳吸附剂，直接在小瓶内解吸减少了不必要的耗时步骤，简化了样品制备方案。
