FAN Er-le,JIANG Xing-yu,ZHANG Jia-dong,et al.Homogeneous Synthesis of Novel Amphiphilic C22 Stationary Phases with Multiple Selectivity[J].Journal of Instrumental Analysis,2023,42(12):1580-1587.
FAN Er-le,JIANG Xing-yu,ZHANG Jia-dong,et al.Homogeneous Synthesis of Novel Amphiphilic C22 Stationary Phases with Multiple Selectivity[J].Journal of Instrumental Analysis,2023,42(12):1580-1587. DOI: 10.19969/j.fxcsxb.23072402.
Homogeneous Synthesis of Novel Amphiphilic C22 Stationary Phases with Multiple Selectivity
In order to solve the variable and irreproducible issues of heterogeneously synthesized chromatographic stationary phases,a new method of homogeneous synthesis was established and used to prepare two newly designed amphiphilic stationary phases,C22-A and C22-A/U,where C22 denotes a long docosyl terminal while U and A denote the strong polar insertions of urea and amide groups at the initial end,respectively. By the means of elemental analysis and nuclear magnetic spectrum,the two new stationary phases contain nitrogen elements,and the ratio of carbon and nitrogen elements accords with the theoretical value,indicating that the amide and urea-based polar groups are successfully bonded to silica gel. Through the chromatographic separation and analysis of the standard sample and the real sample,the shielding effect on upported silicon hydroxyl,hydrophobic selectivity,shape selectivity and hydrophilicity of the two new stationary phases were investigated. It is confirmed that the two new stationary phases have amphiphilic properties as reversed-phase liquid chromatography(RPLC) and hydrophilic interaction chromatography(HILIC). Compared with C18 stationary phases,C22-A and C22-A/U own better shape selectivity,and the double embedded polar groups greatly reduce the silica hydroxyl activity of the stationary phase. C22-A and C22-A/U were used for the separation of several alkaline compounds and estrone(ketone) compounds. The C22 stationary phase solved the problem of serious tailing or insufficient retention of alkaline compounds in the traditional C18 alkyl stationary phase,and successfully realized the separation of estrone(ketone) compounds.
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