State Key Laboratory of Marine Environmental Science, Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystem, College of the Environment and Ecology, Xiamen University, Xiamen 361005, China.
State Key Laboratory of Marine Environmental Science, Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystem, College of the Environment and Ecology, Xiamen University, Xiamen 361005, China.
Talanta. 2015 Mar;134:89-97. doi: 10.1016/j.talanta.2014.10.059. Epub 2014 Nov 6.
In this work, a simple, efficient and environmentally friendly method-multiple monolithic fiber solid-phase microextraction (MMF-SPME) combining with high-performance liquid chromatography (HPLC) was first established for the determination of six trace nitrophenols in water samples. In order to prepare MMF-SPME, 1-allyl-3-methylimidazolium bis [(trifluoro methyl) sulfonyl] imide was co-polymerized with ethylene dimethacrylate to get single thin fiber (0.5 mm in diameter). Subsequently, four thin fibers were bound together to obtain the MMF-SPME. The effect of preparation conditions of MMF-SPME on the extraction performance was investigated in detail. In order to obtain the optimal extraction conditions of MMF-SPME for nitrophenols, several extractive parameters, including desorption solvent, extraction and desorption time, pH values and ionic strength in sample matrix were optimized. Under the optimum conditions, the linear ranges of 4-nitrophenol, 2,4-dinitrophenol, 5-methyl-2-nitrophenol, 5-methoxyl-2-nitrophenol were 0.5-200 µg/L and 1.0-200 µg/L for 2-nitrophenol and 4-tertbutyl-2-nitrophenol. The limits of detection (S/N=3) for the target analytes were 0.075-0.27 µg/L. At the same time, excellent method reproducibility was achieved in terms of intra- and inter-day precisions, indicated by the RSDs of both <10.0%, respectively. Finally, the proposed method was successfully used to detect nitrophenols in different environmental water samples. Satisfactory recoveries ranged from 82.6% to 116% and the RSDs for reproducibility were less than 10% for target analytes in all real samples.
在这项工作中，首次建立了一种简单、高效、环保的方法——多根整体纤维固相微萃取（MMF-SPME）结合高效液相色谱（HPLC），用于测定水样中的六种痕量硝基酚。为了制备 MMF-SPME，将 1-烯丙基-3-甲基咪唑双[(三氟甲基)磺酰]亚胺与乙二醇二甲基丙烯酸酯共聚得到单根细纤维（直径 0.5 毫米）。随后，将四根细纤维绑在一起得到 MMF-SPME。详细研究了 MMF-SPME 的制备条件对萃取性能的影响。为了获得 MMF-SPME 对硝基酚的最佳萃取条件，优化了几种萃取参数，包括解吸溶剂、萃取和解吸时间、样品基质中的 pH 值和离子强度。在最佳条件下，4-硝基苯酚、2,4-二硝基苯酚、5-甲基-2-硝基苯酚、5-甲氧基-2-硝基苯酚的线性范围为 0.5-200 µg/L 和 1.0-200 µg/L 2-硝基苯酚和 4-叔丁基-2-硝基苯酚。目标分析物的检出限（S/N=3）为 0.075-0.27 µg/L。同时，该方法在日内和日间精密度方面表现出优异的重现性，RSD 均<10.0%。最后，该方法成功用于检测不同环境水样中的硝基酚。在所有实际样品中，目标分析物的回收率在 82.6%至 116%之间，重现性的 RSD 小于 10%。
