Shandong Provincial Key Laboratory of Fluorine Chemistry and Chemical Materials, School of Chemistry and Chemical Engineering, University of Jinan, Jinan 250022, China.
Shandong Provincial Key Laboratory of Fluorine Chemistry and Chemical Materials, School of Chemistry and Chemical Engineering, University of Jinan, Jinan 250022, China.
J Chromatogr A. 2022 Sep 13;1680:463428. doi: 10.1016/j.chroma.2022.463428. Epub 2022 Aug 19.
Fluorous affinity chromatography has received growing attention in separation and purification of fluoro compounds, but the wettability of the fluorinated stationary phases is seldom noticed. Here, we construct a series of micro-sized fluorine-containing microspheres by solvothermal precipitation polymerization. The fluorinated microspheres could be obtained with narrow size distribution at even high monomer loading of 15 wt%. Through alternating fluoro monomer, both the particle size and the wettability of the microsphere array could be tuned. Among them, the poly(divinylbenzene -dodecafluoroheptyl methacrylate), P(DVB-DFHMA), microsphere (6.1 μm) arrays displays superhydrophobicity with 153.2° water contact angle. The P(DVB-DFHMA) fluorinated microspheres (7.58% fluorine content) can be packed into steel-less columns as stationary phase for high-performance liquid chromatography. The retention mechanism of the fluorinated column is proven to be the specific fluorine-fluorine interaction. Compared to the commercial C18 silica column, the fluorinated column can completely separate fluorine-containing compounds under high water content mobile phase, including small fluoro molecules and fluoro macromolecules, at much lower back pressure by fluorous affinity.
氟亲和色谱在氟化合物的分离和纯化中受到越来越多的关注，但氟固定相的润湿性很少被注意到。在这里，我们通过溶剂热沉淀聚合构建了一系列微尺度含氟微球。即使在单体负载高达 15wt%的情况下，也可以得到具有窄粒径分布的氟化物微球。通过交替使用氟单体，可以调整微球阵列的粒径和润湿性。其中，聚(二乙烯基苯-全氟庚基甲基丙烯酸酯)，P(DVB-DFHMA)，微球(6.1μm)阵列显示出超疏水性，水接触角为 153.2°。具有 7.58%氟含量的 P(DVB-DFHMA)氟化物微球可填充到无钢柱中作为高效液相色谱的固定相。证明氟化物柱的保留机制是特定的氟-氟相互作用。与商业 C18 硅胶柱相比，氟化物柱在高含水量的流动相下，通过氟亲和作用，在更低的背压下，可完全分离含氟化合物，包括小氟分子和氟大分子。
