基于二茂铁独特的分子结构及其作为新型液相色谱分离基质的潜质,制备了新型(4-环戊二烯基苯甲酸-铁-甲苯)六氟磷酸盐键合硅胶固定相,利用红外光谱、元素分析、热重分析等手段对其进行了表征.分别选取多环芳烃、萘胺位置异构体、硝基苯胺位置异构体、硝基咪唑类化合物和有机磷化合物溶质作为探针,对其色谱性能进行了评价.结果表明,该色谱固定相能提供 π-电子转移、π-π 作用、偶极-偶极作用及与底物的静电相互作用等多种作用力,并探讨了可能的分离机理.
Based on the unique molecular structure of ferrocene and its potential as a new liq-uid chromatography separation medium,a new silica-bonded(4-cyclopentadienyl benzoic acid-iron-toluene)hexafluorophosphoric acid stationary phase was prepared. The structure of this new material was characterized by infrared spectroscopy,elemental analysis,thermogravimet-ric analysis et al. The chromatographic performance and retention mechanism of this new sta-tionary phase were evaluated using different solute probes,including polycyclic aromatic hydro-carbons( PAHs ),positional isomers of naphthylamine,positional isomers of nitro-aniline, nitroimidazoles,organic phosphorus et al. It could provide various action sites for different sol-utes in normal-phase chromatography such as π electron transfer,π-π electron interactions, dipole-dipole interactions,and electrostatic interactions with the substrates. And the possible separation mechanisms are discussed.
参考文献
[1] | Fernandes, C.;Tiritan, M.E.;Pinto, M..Small molecules as chromatographic tools for HPLC enantiomeric resolution: Pirkle-type chiral stationary phases evolution[J].Chromatographia,201315/16(15/16):871-897. |
[2] | Huai QY.;Wang XL.;Zuo YM..Synthesis and evaluation of a ferrocene-bonded silica phase for reversed-phase high-performance liquid chromatography[J].Chromatographia,20029/10(9/10):549-553. |
[3] | Huai QY.;You JM.;Wang Q.;Zuo YM..Evaluation of the retention characteristics of ferrocene-bonded silica stationary phase and other silica-based reversed phases for HPLC using linear solvation energy relationships[J].Chromatographia,200311/12(11/12):709-713. |
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