Chen Xiaoming, Qin Feng, Liu Yueqi, Kong Liang, Zou Hanfa
National Chromatographic Research & Analysis Center, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian, China.
Electrophoresis. 2004 Aug;25(16):2817-24. doi: 10.1002/elps.200405904.
A positively charged chiral stationary phase (CSP) was prepared by chemically immobilizing cellulose 3,5-dimethylphenylcarbamate onto methacryloyldiethylenetriaminopropylated silica (MCDEAPS) via a radical copolymerization reaction. The prepared CSP was evaluated for enantiomer separation in nonaqueous capillary electrochromatography (CEC). Electroosmotic flow (EOF) generated on the prepared CSP could be significantly improved with introduction of positive charges into the CSP, and separation of enantiomers in CEC has been achieved with mobile phases of ethanol and hexane-ethanol, respectively. In addition, we investigated the solvent versatility of the immobilized CSP on enantioseparations in CEC and capillary liquid chromatography (CLC) due to the elimination of dissolution of chiral selector in a number of solvents. Chiral resolution of some enantiomers was improved by adopting tetrahydrofuran (THF) and chloroform as mobile-phase modifiers, respectively.
通过自由基共聚反应将纤维素3,5-二甲基苯基氨基甲酸酯化学固定在甲基丙烯酰二乙烯三胺丙基化硅胶(MCDEAPS)上,制备了带正电荷的手性固定相(CSP)。对制备的CSP进行了非水毛细管电色谱(CEC)对映体分离评价。通过向CSP引入正电荷,可显著改善制备的CSP上产生的电渗流(EOF),并且分别使用乙醇和己烷 - 乙醇流动相在CEC中实现了对映体的分离。此外,由于消除了手性选择剂在多种溶剂中的溶解,我们研究了固定化CSP在CEC和毛细管液相色谱(CLC)对映体分离中的溶剂通用性。分别采用四氢呋喃(THF)和氯仿作为流动相改性剂,提高了一些对映体的手性拆分效果。