低温条件对高效液相色谱手性拆分柱效和选择性的影响  

Column Efficiency and Selectivity in HPLC Chiral Separation at Low Temperature

作　　者：徐丽芳 陈怡 陶建伟 夏寅寅 宋巍 许旭 

机构地区：[1]上海应用技术大学化学与环境工程学院,上海201418

出　　处：《分析科学学报》2016年第4期467-470,共4页Journal of Analytical Science

基　　金：上海市自然科学基金(No.15ZR1440800);上海应用技术学院人才引进科研启动基金(No.YJ2009-21)

摘　　要：本文研究了低温条件下温度对高效液相色谱手性拆分的影响。以消旋安息香为样品,以正己烷-乙醇(70∶30,V/V)为流动相,分别用粒径为3μm、5μm、10μm的Chiralcel OD手性柱,分别在-40℃、-25℃、-10℃、5℃、20℃、35℃柱温条件下,测定了不同流速下安息香手性拆分的保留时间和柱效。根据van Deemter方程对每个温度条件下的H-u关系图进行非线性拟合,得到A、B和C三个系数与温度的关系曲线。根据手性拆分的热力学关系式,在-40℃到35℃柱温范围内,考察各色谱柱对安息香分离的lnk2′-1/T、lnα-1/T的关系均为线性。结果显示,在整个实验温度范围内,安息香在Chiralcel OD手性柱的手性拆分机理不变,降低温度能提高手性分离的选择性,但是会降低通常流速下的柱效,从而影响分离度。随着温度的降低,各色谱柱得到的van Deemter方程中系数A基本不变,系数C随着温度降低逐渐升高。This paper presents the temperature effect on HPLC ehiral separation at low temperature. Using racemic benzoin as target sample, and n-hexane-ethanol （70 ： 30, V/V） as mobile phase, the HPLC chiral separation experiments were conducted at column temperatures of - 40 ℃, - 25 ℃, - 10 ℃, 5 ℃, 20 ℃, and 35 ℃ ,respectively. The retention time and column efficiency were determined at different flow rate （u） using 3 μm, 5 tam,and 10 μm Chiralcel OD columns,respectively. The H-u curves of experiment at each temperature were fitted to obtain the constant A,B and C in van Deemter equation. The relationships between A,B,C terms and temperature were then displayed as A-T, B-T, and C-T curves, respectively. According to the thermodynamics theory of chiral resolution, the lrk′12-1/T,lnα-1/T plots of benzoin chiral separation were drawn and presented linear in the column temperature ranged from -40 ℃ to 35 ℃. The result showed that the benzoin chiral separation mechanism remained the same in the whole tested temperature range in the experiment. Lower temperature can improve the selectivity of the chiral separation, but it reduces the column efficiency. The resolution is then affected. Along with the decrease of the column temperature,in van Deemter equation,A term did not chang basically and C term increased, which are consistent with theory prediction. The result suggests that improving column efficiency is important if lower temperature is used in chiral separation.

关 键 词：高效液相色谱 低温 手性分离 柱效 

分 类 号：O657.72[理学—分析化学]