François Isabelle, Sandra Pat
Ghent University, Department of Organic Chemistry, Krijgslaan 281 (S4-bis), B-9000 Ghent, Belgium.
J Chromatogr A. 2009 May 1;1216(18):4005-12. doi: 10.1016/j.chroma.2009.02.078. Epub 2009 Mar 5.
The separation of the phenacyl esters of the fatty acids originating from a fish oil extract by means of a comprehensive analysis using silver-ion (SI) supercritical fluid chromatography (SFC) and reversed phase liquid chromatography (RP-LC) in the first and second dimensions, respectively, is described. The combination ensured a high orthogonality and peak capacity, particularly when compared to the comprehensive RP-LC x 2RP-LC separation achieved by using a configuration with two columns in parallel in the second dimension. The construction of the SI-SFC x RP-LC interface consists of two two-position/ten-port switching valves, of which one is equipped with two loops packed with octadecyl silica (ODS) particles. Compared to the SFC x RP-LC configuration described in an earlier publication, the peak capacity in the second dimension was increased. Water was not only added as make-up fluid to the SFC effluent to ensure analyte focusing, but also as rinsing medium of the loops prior to the transfer of the fractions to the second dimension. In the SFC dimension, high efficiency and loadability were obtained by coupling two wide-bore columns (4.6 mm ID) in series. Evaporative light scattering (ELSD) and ultraviolet (UV) detection with standard and high-pressure flow cells were evaluated in terms of data acquisition speed and suppression of signal interferences originating from the supercritical carbon dioxide (CO(2)) expansion.
描述了通过分别在第一维和第二维使用银离子（SI）超临界流体色谱（SFC）和反相液相色谱（RP-LC）进行综合分析，分离源自鱼油提取物的脂肪酸苯甲酰酯的方法。这种组合确保了高正交性和峰容量，特别是与通过在第二维使用两根平行柱的配置实现的综合RP-LC×2RP-LC分离相比。SI-SFC×RP-LC接口的构造由两个二位/十通切换阀组成，其中一个配备有两个填充十八烷基硅胶（ODS）颗粒的定量环。与早期出版物中描述的SFC×RP-LC配置相比，第二维的峰容量有所增加。水不仅作为补充流体添加到SFC流出物中以确保分析物聚焦，而且在将馏分转移到第二维之前作为定量环的冲洗介质。在SFC维度中，通过串联两根宽口径柱（内径4.6 mm）获得了高效率和负载能力。根据数据采集速度和对源自超临界二氧化碳（CO₂）膨胀的信号干扰的抑制，对使用标准和高压流通池的蒸发光散射（ELSD）和紫外（UV）检测进行了评估。
