- 期刊
固定相18：逆相液態層析用苯基作尾基之寡聚1,8-雙（二甲基矽基）辛烷固定相之性質及選擇性
Stationary Phases 18: Properties and Selectivity of Linear Oligomeric 1,8-Bis(dimethylsilyl)octane Stationary Phases with Phenyl Ligand as Terminal Group in Reversed-Phase Liquid Chromatography
摘要
本文以1,8-雙（氯二甲基矽基）辛烷與矽膠作用合成寡聚1,8-雙（二甲基矽基）辛烷固定相（RP-PD8），再以苯基二甲基氯矽烷，二苯基甲基氯矽烷集三苯基氯矽烷三種不同苯基數目之矽烷化合物，鍵結於RP-PD8上，可合成三個以苯基作尾基的寡聚1,8-雙（二甲基矽基）辛烷固定相（RP-PD8-MP, RP-PD8-DP,及RP-PD8-TP）。在此三個固定相管柱中，本文分別用芳香物，脂肪物、酮基香香物、硝基芳香物等測試了該逆相液態層析性質，並同時和商用RP-18及自製經三甲基氯矽烷end-capped之寡聚1,8-雙（二甲基矽基）辛烷固定相（RP-PD8-E）作了比較。一般而言，在苯基作尾基之固定相上其滯留行為可發現對變換溶劑含量比例較飽和烷基固定相上更為敏感。極性之溶質諸如一些硝基芳香物或酮基芳香物較偏愛滯留於此類固定相上，但同時對飽和烷基固定相上之滯留則不佳。對各固定相之層析選擇亦用一系列之多環芳香物、烷基苯類、硝基苯類或酮基芳香物評估之，結果顯示，用苯基作尾基之固定相與RP-18及RP-PD8-E比較下頗具選擇性。
關鍵字
無資料並列摘要
A method for the preparation of linear oligomeric 1,8-bis(dimethylsilyl)octane stationary phase (RP-PD8) with phenyldirnethylsilyl, diphenylmethylsilyl or triphenylsilyl ligand (RP-PD8-MP, RP-PD8•DP or RP-PD8-TP) as terminal group was described. Reversed-phase liquid chromatographic properties of these prepared stationary phases were investigated by use of various aromatics, aliphatics, keto-aromatics, nitroaromatics etc. and compared with those of a RP-18 or a end-capped linear oligomeric 1,8-bis(dimethylsilyl)octane phase (RP-PD8-E). In general, retentions on stationary phases with phenyl functionality as terminal group were found to be more sensitive to solvent changes than on saturated phases. Polar solutes such as some nitroaromatics or keto-aromatics were preferentially retained on these prepared phases and rejected on saturated stationary phases. Chromatographic selectivity of each phase was also evaluated by elution of a number of standard mixtures containing poly-aromatics, alkylbenzenes, nitrobenzenes or keto-aromatics. The results suggest that sationary phases with phenyl group as terminal group are found to exhibit a selectivity comparable with both RP-18 and RP-PD8-E.