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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(5μm,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 high performance liquid chromatographic method for the separation of 2-phenylpropionic acid enantiomers using C18 reversed-phase column and hydroxypropyl-β-cyclodextrin as chiral mobile phase additive. Methods: The effects of the concentration of hydroxypropyl-β-cyclodextrin, the mobile phase pH, the proportion of methanol in the mobile phase, the mobile phase flow rate and the column temperature on the chiral separation were investigated. The effects of hydroxypropyl β-cyclodextrin was used to separate the enantiomers of 2-phenylpropionic acid and the calculation of the entrapment constant. The chromatographic conditions were YMC-Pack ODS-A C18 (5μm, 150 mm × 4.6 mm) The phase consisted of 0.5% acetic acid (pH 4.0, adjusted with triethylamine) containing 25 mmol.L -1 hydroxypropyl-β-cyclodextrin-methanol (85:15, v / v) at a flow rate of 0.8 mL.min -1 The column temperature was 45 ℃ and UV detection wavelength was 254 nm. Results: The retention times of (R, S) -2-phenylpropionic acid were 15.85 min and 17.57 min, respectively, and the resolution was 1.50. Conclusion: The method has good separation, simple and easy to operate, and economy than the chiral stationary phase.