Application and comparison of high performance liquid chromatography and high speed counter-current chromatography in enantioseparation of (¡À)-2-phenylpropionic acid

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• 作者：Shengqiang Tong ; Ye Zheng ; Jizhong Yan ; ^{zyx@zjut.edu.cn}
• 关键词：Preparative enantioseparation ; High performance liquid chromatography ; High speed counter-current chromatography ; Hydroxypropyl-¦Â-cyclodextrin ; 2-Phenylpropionic acid
• 刊名：Journal of Chromatography A
• 出版年：2013
• 出版时间：15 March, 2013
• 年：2013
• 卷：1281
• 期：Complete
• 页码：79-86
• 全文大小：537 K

文摘

High performance liquid chromatography (HPLC) and high speed counter-current chromatography (HSCCC) were applied and compared in enantioseparation of 2-phenylpropionic acid (2-PPA) when hydroxypropyl-¦Â-cyclodextrin (HP-¦Â-CD) was used as chiral mobile phase additive. For HPLC, the enantioseparation was achieved on ODS C₁₈ reverse phase column and the mobile phase was 25 mmol L^?1 HP-¦Â-CD aqueous buffer solution (pH4.0, adjusted with triethylamine): methanol: glacial acetic acid (85:15:0.5 (v/v/v)). For HSCCC, the two-phase solvent system was composed of n-hexane-ethyl acetate-0.1 mol L^?1 phosphate buffer solution pH2.67 (5:5:10 for isocratic elution and 8:2:10 for recycling elution (v/v/v)) added with 0.1 mol L^?1 HP-¦Â-CD. The key parameters, such as a substitution degree of HP-¦Â-CD, the concentration of HP-¦Â-CD, pH value of the aqueous phase and the temperature were optimized for both separation methods. Using the optimum conditions a complete HSCCC enantioseparation of 40 mg of 2-propylpropionic acid in a recycling elution mode gave 15-18 mg of (+)-2-PPA and (-)-2-PPA enantiomers with 95-98 % purity and 85-93 % recovery.