State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing 100085, China.
J Chromatogr A. 2012 Mar 23;1230:8-14. doi: 10.1016/j.chroma.2012.01.052. Epub 2012 Jan 25.
A novel approach was developed for the fabrication of solid-phase microextraction (SPME) fiber by coating stainless steel fiber with a polymeric ionic liquid (PIL) through covalent bond. The stainless steel fiber was sequentially coated with a gold film by replacement reaction between Fe and Au when immerged in chloroauric acid, assembled with a monolayer of 3-(mercaptopropyl) triethoxysilane on the gold layer through the Au-S bond, and coated with a silica layer by the hydrolysis and polycondensation reaction of the surface-bonded siloxane moieties and the active silicate solution. Then, 1-vinyl-3-(3-triethoxysilylpropyl)-4,5-dihydroimidazolium chloride ionic liquid was anchored on the silica layer by covalent bond, and the PIL film was further formed by free radical copolymerization between 1-vinyl-3-(3-triethoxysilylpropyl)-4,5-dihydroimidazdium and vinyl-substituted imidazolium with azobisisobutyronitrile (AIBN) as initiator. Parameters influencing the preparation of PIL fiber were optimized, and the developed SPME fiber has a coating thickness of ~20 μm with good thermal stability and long lifetime. The performance of the PIL fiber was evaluated by analysis of polycyclic aromatic hydrocarbons (PAHs) in water samples. The developed PIL fiber showed good linearity between 0.5 and 20 μg l(-1) with regression coefficient in the range of 0.963-0.999, detection limit ranging from 0.05 to 0.25 μg l(-1), and relative standard deviation of 9.2-29% (n=7). This developed PIL fiber exhibited comparable analytical performance to commercial 7 μm thickness PDMS fiber in the extraction of PAHs. The spiked recoveries for three real water samples at 0.5-5 μg l(-1) levels were 49.6-111% for the PIL fiber and 40.8-103% for the commercial PDMS fiber.
开发了一种新方法，通过共价键将聚合离子液体 (PIL) 涂覆在不锈钢纤维上来制备固相微萃取 (SPME) 纤维。不锈钢纤维通过在氯金酸中浸泡时 Fe 与 Au 之间的取代反应被依次涂覆一层金膜，通过 Au-S 键在金层上组装一层 3-(巯丙基)三乙氧基硅烷单层，并通过水解和缩聚反应涂覆一层硅氧烷表面结合的硅烷部分和活性硅酸盐溶液。然后，1-乙烯基-3-(3-三乙氧基硅丙基)-4,5-二氢咪唑氯离子液体通过共价键固定在硅氧烷层上，PIL 薄膜通过 1-乙烯基-3-(3-三乙氧基硅丙基)-4,5-二氢咪唑与乙烯基取代咪唑的自由基共聚与偶氮二异丁腈 (AIBN) 作为引发剂进一步形成。优化了影响 PIL 纤维制备的参数，所开发的 SPME 纤维具有约 20 μm 的涂层厚度，具有良好的热稳定性和长寿命。通过分析水样中的多环芳烃 (PAHs) 来评估 PIL 纤维的性能。所开发的 PIL 纤维在 0.5 至 20 μg l(-1) 之间表现出良好的线性关系，相关系数在 0.963 至 0.999 范围内，检测限范围为 0.05 至 0.25 μg l(-1)，相对标准偏差为 9.2-29%（n=7）。与商业 7 μm 厚 PDMS 纤维相比，该开发的 PIL 纤维在萃取 PAHs 方面具有相当的分析性能。对于三个实际水样在 0.5-5 μg l(-1) 水平的加标回收率，PIL 纤维为 49.6-111%，商业 PDMS 纤维为 40.8-103%。
