合成了一种耐高温的3,4-二(3-苯氧基-4-氟苯基)-2,5-二苯基苯基接枝聚硅氧烷(DPFP)固定相,使用静态涂渍法将其涂渍到毛细管柱内壁上,制成气相色谱柱.分离裂解乙烯的色谱图显示DPFP固定相在360 ℃时仍具有良好的分离能力.DPFP固定相的柱效为3324块/米(保留因子(k)4.24,萘,0.25 mm i.d.).麦克雷诺常数计算结果显示DPFP固定相属中等极性.溶剂化参数模型结果显示DPFP固定相与溶质之间的主要作用力为偶极-诱导偶极作用力、氢键碱性作用力.Grob试剂分离结果显示DPFP色谱柱具有良好的选择性与惰性.另外,芳香族同分异构体、苯取代物、多环芳烃、脂肪酸酯及脂肪醇都得到了良好的分离,表明DPFP固定相在应用方面有巨大的潜力.
A new high-temperature stationary phase called 3,4-di(3-phenoxy-4-fluoro phenyl)-2,5-diphenyl phenyl grafted polysiloxane (DPFP) was synthesized and statically coated on fused-silica capillary columns.The chromatogram of the polyethylene pyrolysis products showed that the DPFP column still owned good separation ability until 360 ℃.The column efficiency of the DPFP was 3324 plates/m (retention factor (k)=4.24, naphthalene, 0.25 mm i.d.).McReynolds constants revealed that the polarity of the stationary phase was moderate.Abraham system constants indicated that DPFP possessed strong dipole-induced dipole interactions and H-bond acceptance with analytes.Analysis of Grob test mixtures showed good selectivity of DPFP and inner-surface inertness of the column.Furthermore, the aromatic isomers, substituted benzenes, polycyclic aromatic hydrocarbons, and fatty acid esters could be well separated on the column, thereby indicating that DPFP had great potential for application.
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