Chen Chunyan, Liang Xiaotong, Wang Jianping, Zou Ying, Hu Huiping, Cai Qingyun, Yao Shouzhuo
State Key Laboratory of Chemo/Biosensing & Chemometrics, College of Chemistry & Chemical Engineering, Hunan University, Changsha 410082, China.
State Key Laboratory of Chemo/Biosensing & Chemometrics, College of Chemistry & Chemical Engineering, Hunan University, Changsha 410082, China.
J Chromatogr A. 2014 Jun 27;1348:80-6. doi: 10.1016/j.chroma.2014.04.098. Epub 2014 May 9.
A novel solid-phase microextraction (SPME) fiber was developed by chemical binding of a crosslinked polymeric ionic liquid (PIL) on the surface of an anodized Ti wire, and was applied in direct-immersion mode for the extraction of perfluorinated compounds (PFCs) from water samples coupled with high performance liquid chromatography-tandem mass spectrometry analysis. The PIL coatings were synthesized by using 1-vinyl-3-hexylimidazolium hexafluorophosphate as monomer and methylacryloyl-substituted polyhedral oligomeric silsesquioxane (POSS) as cross-linker via free radical reaction. The proposed fiber coating exhibited high mechanical stability due to the chemical bonding between the coating and the Ti wire surface. The integration of POSS reagent enhanced the organic solvent resistance of the coating. The parameters affecting the extraction performance of the fiber coating including extraction time, pH of solution, ionic strength and desorption conditions were optimized. The developed PIL-POSS fiber showed good linearity (R<0.998) between 0.1 and 50ngmL(-1) with method detection limits ranging from 0.005 to 0.08ngmL(-1) depending on the analyte, and with relative standard deviation for single-fiber repeatability and fiber-to-fiber reproducibility less than 8.6% and 9.5%, respectively.
通过将交联聚合离子液体（PIL）化学结合在阳极氧化钛丝表面，开发了一种新型固相微萃取（SPME）纤维，并将其以直接浸入模式应用于从水样中萃取全氟化合物（PFCs），同时结合高效液相色谱 - 串联质谱分析。以1 - 乙烯基 - 3 - 己基咪唑六氟磷酸盐为单体，甲基丙烯酰基取代的多面体低聚倍半硅氧烷（POSS）为交联剂，通过自由基反应合成PIL涂层。由于涂层与钛丝表面之间的化学键合，所提出的纤维涂层表现出高机械稳定性。POSS试剂的加入增强了涂层的耐有机溶剂性。对影响纤维涂层萃取性能的参数，包括萃取时间、溶液pH值、离子强度和解吸条件进行了优化。所开发的PIL - POSS纤维在0.1至50 ng mL⁻¹之间显示出良好的线性（R>0.998），方法检测限根据分析物在0.005至0.08 ng mL⁻¹之间，单纤维重复性和纤维间重现性的相对标准偏差分别小于8.6%和9.5%。
