毛细管气相色谱法分离2-苯基羧酸酯对映体  

Enantioseparation of 2-phenylcarboxylic acid esters by capillary gas chromatography

作　　者：史雪岩[1] 刘飞鹏[2] 边庆花[2] 

机构地区：[1]中国农业大学农学与生物技术学院,北京100193 [2]中国农业大学理学院,北京100193

出　　处：《色谱》2016年第1期85-88,共4页Chinese Journal of Chromatography

基　　金：公益性行业(农业)科技专项(201303027)~~

摘　　要：手性2-芳基羧酸酯是制备手性非甾体抗炎药物2-芳基羧酸的重要的中间体,为了建立可用于2-苯基羧酸酯对映体分离的手性毛细管气相色谱法(CGC),分别使用2,6-二-O-戊基-3-O-丁酰基-β-环糊精及2,6-二-O-苄基-3-O-庚酰基-β-环糊精作毛细管气相色谱手性固定相,研究了其对2-苯基丁酸甲酯、2-苯基丁酸乙酯、2-苯基丁酸异丙酯、2-苯基丙酸甲酯及2-苯基丙酸环戊酯等5种2-苯基羧酸酯对映体的分离能力。结果表明,用2,6-二-O-戊基-3-O-丁酰基-β-环糊精及2,6-二-O-苄基-3-O-庚酰基-β-环糊精作手性固定相的毛细管气相色谱法可以分离2-苯基丁酸甲酯、2-苯基丙酸甲酯和2-苯基丙酸环戊酯对映体。2,6-二-O-戊基-3-O-丁酰基-β-环糊精对3种2-苯基羧酸酯对映体的分离能力超过了2,6-二-O-苄基-3-O-庚酰基-β-环糊精。Chiral 2-arylcarboxylic acid derivatives are important intermediates for preparing 2- arylcarboxylic acids, which are non-steroidal anti-inflammatory drugs （NSAIDs）. In order to separate 2-phenylcarboxylic acid ester enantiomers by capillary gas chromatography （ CGC）, 2, 6-di-O-pentyl-3-O-butyryl-fl-cyclodextrin and 2,6-di-O-benzyl-3-O-heptanoyl-fl-cyclodextrin were used as CGC chiral stationary phases, separately, and their enantioseparation abilities to enan- tion/ers of methyl 2-phenylbutanoate, ethyl 2-phenylbutanoate, isopropyl 2-phenylbutanoate, methyl 2-phenylpropionate and cyclopentyl 2-phenylpropionate were examined. It was found that methyl 2-phenylbutanoate, methyl 2-phenylpropionate and cyelopentyl 2-phenylpropionate were successfully separated by using 2,6-di-O-pentyl-3-O-butyryl-fi-cyclodextrin and 2,6-di-O- benzyl-3-O-heptanoyl-β-cyclodextrin as CGC chiral stationary phases, respectively. The enanti- omer separation abilities of 2,6-di-O-pentyl-3-O-butyry-β-cyclodextrin to the three pairs of 2- phenylcarboxylic acid esters tested are superior to those of 2,6-di-O-benzyl-3-O-heptanoyl-β- cyclodextrin.

关 键 词：毛细管气相色谱 Β-环糊精衍生物 手性固定相 2-苯基羧酸酯 对映体分离 

分 类 号：O658[理学—分析化学]