Application and comparison of high performance liquid chromatography and high speed counter-current chromatography in enantioseparation of (±)-2-phenylpropionic acid
Application and comparison of high performance liquid chromatography and high speed counter-current chromatography in enantioseparation of (±)-2-phenylpropionic acid
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高效液相色谱与高速逆流色谱在(±)-2-苯基丙酸对映体分离中的应用及比较
DOI：
10.1016/j.chroma.2013.01.056
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发表时间：
2013-03-15
影响因子：
4.1
通讯作者：
Yan, Jizhong
中科院分区：
文献类型：
--
作者：
Tong, Shengqiang;Zheng, Ye;Yan, Jizhong
以羟丙基- β -环糊精（hp - β - cd）为手性流动相添加剂，采用高效液相色谱（HPLC）和高速逆流色谱（HSCCC）对2-苯基丙酸（2-PPA）的对映体分离进行了比较。HPLC：对映体分离采用ODS C-18反相色谱柱，流动相为25 mmol L-1 hp - β - cd缓冲水溶液（pH4.0，用三乙胺调节）：甲醇：冰醋酸（85:15:5 .5 (v/v/v)）。对于HSCCC，两相溶剂体系由正己烷-乙酸乙酯-0.1 mol L-1磷酸缓冲液pH2.67（等温洗脱为5:5:10，循环洗脱为8:2:10 (v/v/v)）加入0.1 mol L-1 hp - β - cd组成。对两种分离方法的关键参数如hp - β - cd取代度、hp - β - cd浓度、水相pH值和温度进行了优化。在最佳条件下，对40 mg 2-丙丙酸进行HSCCC对映体分离，得到15-18 mg (+)-2- ppa和(-)-2- ppa对映体，纯度为95-98%，回收率为85-93%。(C) 2013 Elsevier B.V.版权所有
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-beta-cyclodextrin (HP-beta-CD) was used as chiral mobile phase additive. For HPLC, the enantioseparation was achieved on ODS C-18 reverse phase column and the mobile phase was 25 mmol L-1 HP-beta-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-beta-CD. The key parameters, such as a substitution degree of HP-beta-CD, the concentration of HP-beta-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. (C) 2013 Elsevier B.V. All rights reserved.