p-取代2-硝基-1-苯乙醇对映体在Chiralcel OD和Chiralpak AD手性柱上的色谱拆分  

Liquid Chromatographic Resolution of p-Substituted 2-nitro-1-phenylethanols on Chiralcel OD and Chiralpak AD Chiral Columns

作　　者：刘慧[1] 胡笛[1] 秦丹丹[1] 陈洪斌[1] 阮源萍[1] 

机构地区：[1]厦门大学化学化工学院,福建厦门361005

出　　处：《厦门大学学报（自然科学版）》2012年第2期219-223,共5页Journal of Xiamen University：Natural Science

基　　金：中央高校基本科研业务费专项基金(2010121014)

摘　　要：为建立准确评价不对称合成反应和手性催化剂的立体选择性分析方法,采用Chiralcel OD-H和Chiralpak AD-H手性柱,研究了7种p-取代2-硝基-1-苯乙醇对映体的高效液相色谱拆分特性.详细考察了手性柱类型、流动相中醇类调节剂对这些对映体色谱拆分行为的影响.结果表明:在优化实验条件下,7种p-取代2-硝基-1-苯乙醇对映体均可达到很好的基线拆分,并且方法简便、准确,适合于不对称亨利反应合成p-取代2-硝基-1-苯乙醇化合物的对映体纯度分析.The enantioseparation of seven pairs of p-substituted 2-nitro-1-phenylethanols was achieved with high performance liquid chromatography by using cellulose tris（3,5-dimethylphenylcarbamate）（Chiralcel OD-H） and amylose tris（3,5-dimethylphenylcarbamate）（Chiralpak AD-H） as chiral stationary phases and hexane-isopropanol or hexane-ethanol as mobile phases in various percentages.The effects of type of chiral stationary phase and alcohol in the mobile phase on the retention and resolution were investigated.On the Chiralcel OD-H column,the enatiomers elute faster with ethanol than with isopropanol modifier as expected from the higher polarity of ethanol.However,on Chiralpak AD-H column the retention factors of all the enantiomers increase,the enantioseparation factors dramatically change on changing isopropanol to ethanol.The enantioseparation on the Chiralpak AD-H column is much more influenced by the kind of alcohol in the mobile phase than the Chiralcel OD-H.Under optimized conditions,baseline enantioseparation of seven pairs of p-substituted 2-nitro-1-phenylethanols were easily obtained.

关 键 词：p-取代2-硝基-1-苯乙醇 对映体拆分 高效液相色谱 手性固定相 

分 类 号：O657.72[理学—分析化学]