目的以羧甲基-倍他-环糊精(CM-β-CD)为手性选择剂,建立新型活性化合物Ⅱ-f对映体的毛细管电泳拆分方法,并对其左旋对映体的过量值(e.e.%值)进行测定。方法采用未涂层熔融石英毛细管柱,背景电解质为Tris-H3PO4缓冲溶液。考察了手性选择剂CM-β-CD浓度、pH值、缓冲溶液浓度、工作电压及温度对对映体分离的影响。结果在优化条件下,即20mmol·L-1CM-β-CD、40mmol·L-1Tris-H3PO4(pH4.4,50%甲醇v/v)的运行缓冲液,分离电压20kV,温度20℃,Ⅱ-f两对映体分离度达3.5,标记出峰顺序为右旋体杂质先出峰,左旋Ⅱ-f粗品与精制品样品的e.e.%值测定结果分别为72.50%和100%。结论该法简单快速,可用于Ⅱ-f对映体的质量控制。
OBJECTIVE This study established an enantioseparation method of novel active compound Ⅱ-f by capillary electrophoresis with CM-β-CD as chiral selector.METHODS The influences of the selector concentration,pH and concentration of buffer solution,applied voltage and temperature were investigated.RESULTS The optimum condition was obtained with 20 kV as separation voltage,20mmol·L-1 CM-β-CD,40mmol·L-1 Tris-H3PO4(pH 4.4),50% methanol(v/v) as running buffer at 20℃.Under optimum condition,baseline separation was achieved between the two enantiomers of Ⅱ-f with the resolution of 3.5,the established method was finally applied to determine the enantiomeric excess value(e.e.% value) of(S)-Ⅱ-f crude product and purification product,the determination result was 72.50% and 100%.CONCLUSION This method is simple and fast,can be adopted in(S)-Ⅱ-f quality control.