摘要
以3-[N,N-二甲基-[2-(2-甲基丙-2-烯酰氧基)乙基]铵]丙烷-1-磺酸内盐(SPE)为功能单体,季戊四醇三丙烯酸酯(PETA)为交联剂,环己醇和乙二醇(EG)为致孔剂,通过原位聚合法制备磺酸甜菜碱型两性离子亲水毛细管整体柱。优化单体、交联剂和致孔剂的比例等因素,考察了不同SPE含量对整体柱性能和选择性的影响。在最优制备条件下,以苯酚类化合物、烷基苯类化合物和苯甲酸类化合物为分离对象,评价该整体柱的色谱性能以及分离机理。在不同的色谱条件下,该整体柱具有亲水、疏水以及离子交换作用。此整体柱在0.05 m L/min的流速下(线速度为0.265 mm/s)分离烷基苯类化合物时,柱效高达41000-56000 plates/m,该整体柱重现性良好,连续运行的重现性(RSD)低于1.2%。在亲水/离子交换色谱模式下,该整体柱可应用于核苷和碱基的高效分离。
Sulfobetaine-based capillary zwitterionic hydrophilic monolithic stationary phase was prepared for cLC by in situ copolymerization of N, N-dimethyl-N-methacryloxyethyl N - (3-sulfopropyl) ammonium betaine (SPE) and pentaerythritol triacrylate (PETA) in a binary porogenie solvent consisting of cyclohexanol and ethyleneglycol. The resultant monoliths with different column properties and selectivity were optimized by adjusting the ratio of SPE to PETA and the composition of porogenic solvent. A series of phenols, alkylbenzenes and cm'boxybenzenes were used to evaluate the column performance in terms of hydrophilic, hydrophobic and cation-exchange interactions. At an optimized flow rate of 50 mL/min (corresponding to 0. 265 mm/s ), the monolith exhibited high column efficiencies of 43,000-56,000 plates/m for alkylbenzenes. Good repeatability was obtained with relative standard deviation (RSD) of retention factor (k) less than 0. 65% for rim-to-run (n =5). The poly (SPE-co-PETA) monolithic column was applied to the separation of nucleotides and nucleobases.
出处
《分析试验室》
CAS
CSCD
北大核心
2016年第12期1445-1450,共6页
Chinese Journal of Analysis Laboratory
基金
福建省自然科学基金项目(2013J01032)
福建省教育厅科研项目(JA15778)资助
关键词
磺酸甜菜碱
两性离子亲水整体柱
制备
毛细管液相色谱(cLC)
Sulfobetaine
Zwitterionic hydrophilic monolithic column
Perpartion
Capillary liquid chromatography ( cLC )