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.
Anal Chim Acta. 2015 Oct 29;899:75-84. doi: 10.1016/j.aca.2015.10.004. Epub 2015 Oct 20.
In this research, the applicability of a new sorbent based on boronate affinity material is demonstrated. For this purpose, six strong polar nitrophenols were selected as models which are difficult to be extracted in neutral form (only based on hydrophobic interactions). The extracted nitrophenols were separated and determined by high-performance liquid chromatography with diode array detection. The sorbent was synthesized by in situ copolymerization of 3-acrylamidophenylboronic acid and divinylbenzene using dimethyl sulfoxide and azobisisobutyronitrile as porogen solvent and initiator, respectively. The effect of the preparation parameters in the polymerization mixture on extraction performance was investigated in detail. The size and morphology of the sorbent have been characterized via different techniques such as infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry. The important parameters influencing the extraction efficiency were studied and optimized thoroughly. Under the optimum extraction conditions, the limits of detection (S/N = 3) and limits of quantification (S/N = 10) for the target nitrophenols were 0.097-0.28 and 0.32-0.92 μg/L, respectively. The precision of the proposed method was evaluated in terms of intra- and inter-assay variability calculated as RSD, and it was found that the RSDs were all below 9%. Finally, the developed method was successfully applied for environmental water samples such as wastewater, tap, lake and river water. The recoveries varied within the range of 71.2-115% with RSD below 11% in all cases. The results well demonstrate that the new boronate affinity sorbent can extract nitrophenols effectively through multi-interactions including boron-nitrogen coordination, hydrogen-bond and hydrophobic interactions between sorbent and analytes.
在这项研究中，展示了一种基于硼酸亲和材料的新型吸附剂的适用性。为此，选择了六种强极性硝基苯酚作为模型，这些模型难以在中性形式下被提取（仅基于疏水相互作用）。提取的硝基苯酚通过高效液相色谱法与二极管阵列检测分离和测定。吸附剂通过 3-丙烯酰胺基苯硼酸和二乙烯基苯的原位共聚合成，分别使用二甲基亚砜和偶氮二异丁腈作为致孔剂溶剂和引发剂。详细研究了聚合混合物中制备参数对萃取性能的影响。通过不同的技术，如红外光谱、元素分析、扫描电子显微镜和压汞孔隙率，对吸附剂的尺寸和形态进行了表征。研究并优化了影响萃取效率的重要参数。在最佳萃取条件下，目标硝基苯酚的检测限（S/N = 3）和定量限（S/N = 10）分别为 0.097-0.28 和 0.32-0.92 μg/L。该方法的精密度通过日内和日间变异系数（RSD）评估，结果表明 RSD 均低于 9%。最后，该方法成功应用于环境水样，如废水、自来水、湖泊和河水。在所有情况下，回收率在 71.2-115%范围内，RSD 低于 11%。结果表明，新型硼酸亲和吸附剂可以通过硼酸-氮配位、氢键和吸附剂与分析物之间的疏水相互作用等多种相互作用有效地提取硝基苯酚。
