【摘要】 目的采用正相手性色谱柱建立莨菪烷衍生物A和B对映体的高效液相色谱法(HPLC)手性分离方法。方法在正相条件下分别使用Chiralpak AD和Chiralcel OD-H手性柱,考察流动相组成、流速和柱温对对映体手性分离的影响;计算对映体与固定相相互作用的焓变差值和熵变差值等热力学参数。结果化合物A在Chiralpak AD柱上得到最佳色谱分离条件。化合物B在Chiralcel OD-H柱上得到最佳色谱分离条件。在15℃~35℃柱温范围内,lnα对1/T呈线性关系,其手性分离过程受焓控制。结论此HPLC手性分离方法可用于化合物A和B的光学纯度分析和鉴定。更多还原

【Abstract】 Objective To develop a high performance liquid chromatography( HPLC) chiral separation method for the enantiomers A and B of tropane derivatives by the normal phase chiral chromatographic column.Methods The chiral columns of Chiralpak ADand Chiralcel O D-H were employed under the normal phase condition.Effects of the composition of mobile phase, flowrate, and temperature on the chiral separation of enantiomers were observed.Thermodynamic parameters of the interaction of enantiomers and stationary phase such as the enthalpy difference and entropy difference were calculated.Results The optimal enantiomeric separation condition for compound A was obtained on the Chiralpak ADcolumn.The optimal enantiomeric separation condition for compound B was obtained on the Chiralcel O D-H column.The lnα was linear with 1/Tbetween 15 ℃ and 35 ℃.The chiral separation was controlled by enthalpy.Conclusion This H PLCchiral separation method can be used for the analysis and identification of optical purity of tropane derivatives A and B.更多还原