Pei Miao, Zhang Zirui, Huang Xiaojia, Wu Yuanfei
State Key Laboratory of Marine Environmental Science, Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystem, The Fujian Provincial Key Laboratory for Coastal Ecology and Environmental Studies, 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, The Fujian Provincial Key Laboratory for Coastal Ecology and Environmental Studies, College of the Environment and Ecology, Xiamen University, Xiamen 361005, China.
Talanta. 2017 Apr 1;165:152-160. doi: 10.1016/j.talanta.2016.12.043. Epub 2016 Dec 21.
A multiple monolithic fiber solid-phase microextraction (MMF-SPME) utilizing polymeric ionic liquid-based adsorbent was prepared. The adsorbent was obtained by in situ copolymerization of an ionic liquid, 1-trimethyl-(4-vinylbenzyl) aminium chloride and dual cross-linkers (divinylbenzene and ethylenedimethacrylate). The effect of preparation conditions including the content of ionic liquid and porogen in the polymerization mixture on extraction performance was studied in detail. Infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry were used to inspect the physicochemical properties of the new adsorbent. The applicability of the new MMF-SPME was demonstrated by the extraction of trace endocrine disrupting chemicals (EDCs). Results indicated that the prepared MMF-SPME could extract EDCs effectively through multi-interactions such as ion-exchange, π-π and hydrophobic interactions. After optimization of extraction parameters, a method of MMF-SPME coupled to high performance liquid chromatography/diode array detection was conducted to detect trace EDCs in complicated samples including environmental water and human urine. The limits of detection (S/N=3) and quantification (S/N=10) for targeted compounds were 0.011-0.065μg/L and 0.036-0.21μg/L, respectively. Satisfactory precision was also achieved by evaluating the repeatability and intermediate precision with relative standard deviations (RSDs) of less than 9% and 10%, respectively. At the same time, the proposed method was successfully applied for the determination of EDCs in water and human urine with spiking recoveries ranged from 70.6% to 119%.
制备了一种利用基于聚合离子液体的吸附剂的多重整体纤维固相微萃取（MMF-SPME）。该吸附剂通过离子液体1-三甲基-（4-乙烯基苄基）氯化铵与双交联剂（二乙烯基苯和乙二醇二甲基丙烯酸酯）原位共聚获得。详细研究了聚合混合物中离子液体和致孔剂含量等制备条件对萃取性能的影响。采用红外光谱、元素分析、扫描电子显微镜和压汞法对新型吸附剂的理化性质进行了考察。通过萃取痕量内分泌干扰化学物质（EDCs）证明了新型MMF-SPME的适用性。结果表明，制备的MMF-SPME可通过离子交换、π-π和疏水相互作用等多种相互作用有效地萃取EDCs。在优化萃取参数后，采用MMF-SPME与高效液相色谱/二极管阵列检测联用的方法检测环境水和人尿等复杂样品中的痕量EDCs。目标化合物的检测限（S/N=3）和定量限（S/N=10）分别为0.011-0.065μg/L和0.036-0.21μg/L。通过评估重复性和中间精密度，相对标准偏差（RSD）分别小于9%和10%，也获得了令人满意的精密度。同时，该方法成功应用于水和人尿中EDCs的测定，加标回收率在70.6%至119%之间。
