去甲万古霉素手性固定相的制备及其对5-甲基-5-苯基乙内酰脲的拆分

Preparation of Norvancomycin Chiral Stationary Phase for the Resolution of 5-Methyl-5-phenylhydantoin

将去甲万古霉素作为手性选择剂键合到硅胶载体上,制备成一种新型的手性固定相,用该手性固定相拆分5-甲基-5-苯基乙内酰脲.在反相和极性有机流动相中,5-甲基-5-苯基乙内酰脲能够被对映分离.考察了反相流动相模式下流动相组成、柱温、缓冲液pH值和体积流量对拆分的影响.在反相模式下,流动相为V(甲醇)∶V(质量分数为2%的三乙胺醋酸(pH5.5))=10∶99,体积流量0.6 mL/min,柱温20℃时能获得很好的拆分效果.

Norvancomycin was covalently bonded to the silica gel as a chiral selector to synthesize a new ehiral stationary phase, NVC-CSP. Enantiomers of 5-Methyl-5-phenylhydantoia （MPH） were separated on the NVC-CSP. MPH may be enantioseparated under the reversed phase and polar organie mode. The effects of composition, column temperature, pH and flow rate of mobile phase on the enantioseparation were investigated. It is shown that the enantioseparation by V （CH3OH） ： V（2% TEAA （pH 5. 5））=10 ： 90 at the flow rate 0. 6 mL/min and 20℃ is excellent.