State Key Laboratory of Marine Environmental Science, College of the Environment and Ecology, Xiamen University, P.O. Box 1009, Xiamen 361005, China.
Anal Bioanal Chem. 2013 Mar;405(7):2185-93. doi: 10.1007/s00216-012-6301-3. Epub 2012 Aug 15.
A novel porous monolith has been prepared and used as a sorbent in stir-cake-sorptive extraction (SCSE). The monolithic material was prepared by in-situ copolymerization of allyl thiourea (AT) and divinylbenzene (DB) in the presence of dimethylformamide as a porogen solvent. To optimize the polymerization conditions, different monoliths with different ratios of functional monomer to porogenic solvent were prepared, and their extraction efficiency was investigated in detail. The monolith was characterized by elemental analysis, scanning electron microscopy, mercury intrusion porosimetry, and infrared spectroscopy. Analysis of polar phenols in environmental water samples by a combination of ATDB-SCSE and HPLC with diode-array detection was selected as a model for the practical application of the new sorbent. Several extraction conditions, including extraction and desorption time, pH, and ionic strength of the sample matrix were optimized. The results showed that the new monolith had high affinity for polar phenols and could be used to extract them effectively. Under the optimum conditions, low detection (S/N = 3) and quantification (S/N = 10) limits were achieved for the phenols, within the ranges 0.18-0.90 and 0.59-2.97 μg L(-1), respectively. The linearity of the method was good, and the method enabled simple, practical, and low-cost extraction of these analytes. The distribution coefficients between ATDB and water (K(ATDB/W)) were calculated for the phenolic compounds and compared with K(O/W). Finally, the proposed method was successfully applied to the determination of the compounds in three environmental water samples, with acceptable recovery and satisfactory repeatability.
一种新型的多孔整体材料已经被制备出来，并作为搅拌饼吸附萃取（SCSE）的吸附剂使用。整体材料是通过在二甲基甲酰胺作为致孔溶剂的存在下，使丙烯硫脲（AT）和二乙烯基苯（DB）原位共聚制备的。为了优化聚合条件，制备了不同功能单体与致孔溶剂比例的不同整体材料，并详细研究了它们的萃取效率。通过元素分析、扫描电子显微镜、压汞法和红外光谱对整体材料进行了表征。采用 ATDB-SCSE 与 HPLC 二极管阵列检测相结合的方法分析环境水样中的极性酚类化合物，作为新型吸附剂实际应用的模型。优化了几个萃取条件，包括萃取和洗脱时间、样品基质的 pH 值和离子强度。结果表明，新型整体材料对极性酚类化合物具有高亲和力，可有效用于萃取。在最佳条件下，酚类化合物的检测限（S/N = 3）和定量限（S/N = 10）分别为 0.18-0.90 μg/L 和 0.59-2.97 μg/L。该方法具有良好的线性，能够简单、实用且低成本地萃取这些分析物。计算了酚类化合物在 ATDB 和水之间的分配系数（K（ATDB/W）），并与 K（O/W）进行了比较。最后，该方法成功应用于三种环境水样中化合物的测定，回收率可接受，重复性好。
