【摘要】 在纤维素-三-(35,-二甲基苯基氨基甲酸酯)(Chiralcel OD-H)手性柱上对硅氟唑对映体的分离进行了研究。考察了流动相中改性剂的种类和浓度、流速以及柱温对分离效果的影响,并对手性拆分机制进行了讨论。实验结果表明:5种醇改性剂中,异丙醇的改性效果最佳,当异丙醇含量为2%时,分离度(Rs)达最大值10.19;在0.4～1.1mL.min-1的流速条件下,分离度(Rs)随着流速的增大而逐渐减小;在15℃～35℃的温度变化范围内,分离因子(α)随温度的升高而呈降低趋势。在柱温为25℃,V(正己烷):V(异丙醇)=85∶15为流动相,流速1.0mL.min-1的条件下,硅氟唑对映体能达到基线分离,分离因子(α)和分离度(Rs)分别为1.69和5.31。更多还原

【Abstract】 Enantiomeric separation of simeconazole enantiomers by high performance liquid chromatography(HPLC) with the coating-type cellulose tris(3,5-dimethylphenylcarbamate)chiral stationary phase(Chiralcel OD-H column)were studied,the enantioselectivity separation mechanism has also been discussed..The effects of chromatographic conditions such as the mobile phase composition including the concentration and type of the alcohol modifiers in mobile phase,flow rate,column temperature on enantiomers separation were considered.The data indicated that isopropanol had a better modified effect than other alcohol modifiers,and two enantiomers was best separated with the resolution(Rs)of 10.19 by 2% isopropanol in mobile phase.The resolution(Rs)of simeconazole was decreased with the flow rate increased in the range of 0.4-1.1 mL·min-1.The effect of temperature on chiral separation was investigated,it was found that higher column temperature resulted in a lower selectivity factor(α)for simeconazole in the temperature range of 15℃-35℃.A baseline separation of the enantiomers was obtained with a mobile phase of n-hexane/isopropanol(85:15 by vol) at a flow rate of 1.0 mL·min-1 under 25 ℃,the selectivity factor(α)and resolution(Rs)was 1.69 and 5.31 respectively.更多还原