Huang Yanmei, Huang Xiaojia
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.
J Chromatogr A. 2017 Apr 7;1492:12-18. doi: 10.1016/j.chroma.2017.03.001. Epub 2017 Mar 3.
A new type of highly fluorinated monolith (HFM) was fabricated and used as adsorbent of multiple monolithic fiber solid-phase microextraction (MMF-SPME). To prepare the HFM, a fluorinated monomer, 2,2,3,3,4,4,5,5,6,6,7,7-dodecafluoroheptyl acrylate was in situ copolymerized with dual cross-linkers (divinylbenzene and ethylenedimethacrylate). The fabrication parameters including the content of monomer and porogenic solvent in the polymerization mixture were optimized to obtain expected extraction performance and life span. The physicochemical properties of the HFM were systematically investigated with elemental analysis, infrared spectroscopy, scanning electron microscopy and mercury intrusion porosimetry. The effective extraction of six fluorobenzenes was selected as a paradigm to demonstrate the fluorophilic characteristic of HFM/MMF-SPME. At the same time, a convenient and effective method for the determination of trace fluorobenzenes in environmental water samples was developed by coupling HFM/MMF-SPME with high performance liquid chromatography/diode array detection (HFM/MMF-SPME-HPLC/DAD). Results indicated that the limits of detection (S/N=3) for targeted compounds were in the range of 1.09-5.88μg/L. The intra-day and inter-day precision (relative standard deviations, n=4, %) at two spiked concentrations were 4.2-10.6% and 6.1-10.8%, respectively. Finally, the developed method was successfully applied to the analysis of fluorobenzenes in spiked real water samples with satisfactory recoveries and repeatability.
制备了一种新型的高氟化整体柱（HFM），并将其用作多整体纤维固相微萃取（MMF-SPME）的吸附剂。为制备HFM，使氟化单体丙烯酸2,2,3,3,4,4,5,5,6,6,7,7-十二氟庚酯与双交联剂（二乙烯基苯和乙二醇二甲基丙烯酸酯）进行原位共聚。对聚合混合物中单体和致孔溶剂的含量等制备参数进行了优化，以获得预期的萃取性能和使用寿命。通过元素分析、红外光谱、扫描电子显微镜和压汞法对HFM的物理化学性质进行了系统研究。选择对六种氟苯的有效萃取作为范例，以证明HFM/MMF-SPME的亲氟特性。同时，通过将HFM/MMF-SPME与高效液相色谱/二极管阵列检测（HFM/MMF-SPME-HPLC/DAD）联用，建立了一种简便有效的测定环境水样中痕量氟苯的方法。结果表明，目标化合物的检测限（S/N=3）在1.09-5.88μg/L范围内。在两个加标浓度下，日内和日间精密度（相对标准偏差，n=4，%）分别为4.2-10.6%和6.1-10.8%。最后，所建立的方法成功应用于加标实际水样中氟苯的分析，回收率和重复性良好。
