分析测试学报2023，Vol.42Issue(12)：1580-1587,8.DOI:10.19969/j.fxcsxb.23072402
均相合成多重选择性的新型两亲性C22高效液相色谱固定相
Homogeneous Synthesis of Novel Amphiphilic C22 Stationary Phases with Multiple Selectivity
摘要
Abstract
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 am-ide 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 nitro-gen 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,hydro-phobic selectivity,shape selectivity and hydrophilicity of the two new stationary phases were investi-gated.It is confirmed that the two new stationary phases have amphiphilic properties as reversed-phase liquid chromatography(RPLC)and hydrophilic interaction chromatography(HILIC).Com-pared with C18 stationary phases,C22-A and C22-A/U own better shape selectivity,and the dou-ble 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)com-pounds.The C22 stationary phase solved the problem of serious tailing or insufficient retention of al-kaline compounds in the traditional C18 alkyl stationary phase,and successfully realized the separa-tion of estrone(ketone)compounds.关键词
色谱固定相/两亲性/均相合成/药物分析/液相色谱Key words
chromatographic stationary phase/amphiphilicity/homogeneous synthesis/drug analysis/liquid chromatography分类
化学化工引用本文复制引用
范二乐,蒋星宇,张加栋,张明亮,韩海峰,张大兵,陈义..均相合成多重选择性的新型两亲性C22高效液相色谱固定相[J].分析测试学报,2023,42(12):1580-1587,8.基金项目
国家自然科学基金重点项目(22134007) （22134007）
