摘要
在碱性条件下合成了单(六-氧-甲基丙烯酸酯)-β-环糊精(CD),以甲基丙烯酸甘油酯(GMA)和单(六-氧-甲基丙烯酸酯)-β-CD为单体,乙二醇二甲基丙烯酸酯(EDMA)为交联剂,2-丙烯酰胺基-2-甲基-1-丙磺酸(AMPS)用来产生电渗流,正丙醇和1,4-丁二醇为制孔剂,偶氮二异丁腈(AIBN)为引发剂,在内径100μm的毛细管内原位聚合制得了手性毛细管电色谱整体柱。采用制得的手性整体柱,在加压毛细管电色谱(pCEC)模式下,对吉培福林对映体进行手性分离,考察了流动相配比、背景电解质pH值、柱温和分离电压等对分离的影响。在缓冲溶液为5mmol/LNaH2PO4-Na2HPO4(pH2.5)、运行电压20kV、毛细管温度15℃条件下,16min内成功分离了吉培福林对映体,其分离度为1.53。
Mono（6-deoxy-methacrylate）-/3-CD was synthesized under alkaline conditions. A chiral capillary monolithic column was prepared in 100 μm i.d. capillary column using 2-acrylamide-2- methylpropanesulfonic acid to produce electroosmotic flow （EOF） with butyl-methacrylate and mono （6-deoxy-methacrylate）-β-CD as monomer, ethylene-glycol-dimethacrylate （EDMA）as cross-linking agent, 1, 4-butanediol and propanol as porogenic agent and azobisihutyronitrile as initiator. Gepe- frine enantiomers were separated on the prepared chiral capillary monolithic column under pressurized capillary electrochromatography （pCEC） mode. The influences of mobile phase ratio, buffer pH, column temperature and applied voltage on resolution were investigated. Results showed that the optimal conditions were as follows： buffer solution concentration was 5 retool/L（ NaH2PO4 -NazHPO4, pH 2.5 ）, separation voltage was 20 kV, and column temperature was 15℃. Under the optimal conditions, gepefrine enantiomers were separated successfully at baseline within 16 min with the resolution of 1.53. This method is promising in the routine analysis on chiral drug in practice.
出处
《分析测试学报》
CAS
CSCD
北大核心
2009年第5期608-610,共3页
Journal of Instrumental Analysis
关键词
吉培福林
毛细管电色谱
手性整体柱
对映体拆分
gepefrine
capillary electrochromatography
chiral monolithic column
enantiomer separation
