某些酚类的高温液相色谱行为  

Liquid Chromatographic Behavior of Some Phenols at Elevated Temperature

作　　者：富玉[1] 宋瑞娟[1] 石宏宇[1] 龙远德[1] 黄天宝[1] 

机构地区：[1]中国科学院成都有机化学研究所

出　　处：《分析化学》2007年第5期727-730,共4页Chinese Journal of Analytical Chemistry

摘　　要：建立了高温液相色谱系统,在高温条件下,采用甲醇-水作为流动相,在Polymerx RP-1聚合物（PS-DVB）色谱柱上考察了6种酚类样品的色谱行为。实验条件：温度40~160℃,流速0.2~5.5mL/min,流动相中甲醇浓度范围40%~80%。考察了温度、流速和流动相组成对酚类样品的保留、分辨、柱效和系统压力的影响,探讨了酚类样品在聚合物柱上的热力学行为。温度升高2.35℃大约相当于流动相中甲醇浓度增加1%,可以通过改变色谱柱温度调节样品保留和改变选择性。柱温升高,降低了流动相的粘度,允许在高温条件下使用较高的流速实现快速分离。在160℃、V（甲醇）∶V（水）=40∶60,为流动相和3mL/min流速条件下,可于2.5min内实现6种酚类的完全分离。A system of high temperature liquid chromatography was established. The chromatographic behavior of some phenols on a Polymerx RP-1 （PS-DVB） column was researched by using methanol-water as the mobile phase with the column temperature of 40 ℃- 160℃, the mobile phase flow rate of 0.2 - 5.5 mL/min and the percentage of methanol in the mobile phase of 40% - 80%. The effects of temperature, flow rate and composition of mobile phase on retention, resolution, column efficiency and the pressure of the system were examined. The thermodynamics of the chromatographic process of the phenols on Polymerx RP-1 column at high temperature was also discussed. It was found that a temperature increase of 2.35 ℃ had approximately the same effect as 1% increase in methanol concentration in the mobile phase. Changing the column temperature allows one to adjust the retention and optimize the chromatographic selectivity. Increasing the column temperature lowers the viscosity of the mobile phase and allows one to actualize rapid analysis at elevated temperature and high flow rate of mobile phase. The separation of six phenolic compounds was achieved within 2.5 min at 160℃ and flow rate of 3 mL/min using methanol-water （40： 60, V/V） as mobile phase.

关 键 词：高温液相色谱 酚类 热力学 保留 柱效 

分 类 号：O625.3[理学—有机化学]