高效液相色谱手性流动相添加法拆分2-苯丙酸对映体

目的: 采用C₁₈反相色谱柱,以羟丙基-β-环糊精作为手性流动相添加剂,建立了2-苯丙酸对映体的高效液相色谱拆分方法。 方法: 考察了羟丙基-β-环糊精的浓度、流动相pH、流动相中甲醇的比例、流动相流速和柱温对手性分离的影响,同时探讨了高效液相色谱采用羟丙基-β-环糊精分离2-苯丙酸对映体的分离机制及包结常数的计算,确定了色谱条件为YMC-Pack ODS-A C₁₈ (5 μm,150 mm×4.6 mm) 色谱柱,流动相为0.5%乙酸 (pH 4.0,三乙胺调节)含25 mmol·L^-1 羟丙基-β-环糊精-甲醇 (85∶15,v/v),流速为0.8 mL·min^-1,柱温为45 ℃,紫外检测波长为254 nm。 结果: (R,S)-2-苯丙酸的保留时间分别为15.85 min和17.57 min,分离度为1.50。 结论: 本方法分离度好,简便易行,且比手性固定相经济。

Objective: To establish a method for enantioseparation of 2-phenylpropionic acid(2-PPA)using high performance liquid chromatography with hydroxypropyl-β-cyclodextrin (HP-β-CD) as the chiral mobile phase additive and a C₁₈ reversed-phase column as the stationary phase. Methods: The influences of the concentration of HP-β-CD,pH value of aqueous phase,methanol content,flow rate and column temperature on the peak resolution were investigated,and the mechanism of inclusion complex between HP-β-CD and 2-phenylpropionic acid was studied by HPLC.The enantiomers separation was carried out on a YMC-Pack ODS-A C₁₈(5 μm,150 mm×4.6 mm) column with chiral mobile phase consisted of 0.5% triethylamine acetate buffer (pH 4.0) containing 25 m mol·L^-1 HP-β-CD-methanol (85∶15,v/v). The detecting wavelength was 254 nm.The flow rate was set at 0.8 mL·min^-1 and the column temperature was 45 ℃. Results: The retention time of R-2-phenylpropionic acid and S-2-phenylpropionic acid were 15.85 min and 17.57 min,and the resolution of 1.50 was achieved. Conclusion: The established method is simple,economic and with a good resolution.

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