Chen J, Huang W, Zhang L, Tian Y
Dalian Institute of Chemical Physics, the Chinese Academy of Scienses, Dalian, 116012.
Se Pu. 1997 May;15(3):222-4.
An on-line coupling system of normal phase microbore HPLC and capillary GC has been established, in which retention gap technique with on-column injection and partially concurrent solvent evaporation with early vapor exit were used. The conditions suitable for the coupling system of HPLC and CGC must be determined experimentally since the factors have to be adjusted with respect to solvent evaporation temperature and column inlet pressure etc. The suitable solvent evaporation temprature for the mobile phase used for this system, n-hexane, was about 70 degrees C. A temperature much, lower or higher than 70 degrees C will influence the GC analysis. In addition, solvent evaporation temperature and column inlet pressure are interacting, that is, higher solvent evaporation temperature needs higher inlet pressure. At the above evaporation temperature, the suitable inlet pressure for this system was about 0.2MPa. In order to minimize the extra-column effect on the LC peaks, thin transfer-line and connectors of zero-dead volume between LC column and GC column must be used. The separation and analysis of aromatics in a light diesel fuel was performed by using this system with 15cm x 2mm i.d. YGW (5microm) silica LC column and 60m x 0.25mm i.d. OV-101 GC column under the above conditions. The analytical results show that the system of on-line coupling of HPLC with CGC is a reliable analytical tool for microcomponents in complex mixtures, especially for those requiring sample preparation prior to GC.
建立了正相微径高效液相色谱(HPLC)与毛细管气相色谱(GC)的在线联用系统,该系统采用柱上进样的保留间隙技术以及早期蒸汽出口的部分同时溶剂蒸发技术。由于必须根据溶剂蒸发温度和柱入口压力等因素进行调整,所以适合HPLC与CGC联用系统的条件必须通过实验来确定。该系统所用流动相正己烷的适宜溶剂蒸发温度约为70℃。温度远低于或高于70℃都会影响GC分析。此外,溶剂蒸发温度和柱入口压力相互影响,即较高的溶剂蒸发温度需要较高的入口压力。在上述蒸发温度下,该系统的适宜入口压力约为0.2MPa。为了使对液相色谱峰的柱外效应最小化,必须使用细的传输线以及液相色谱柱和气相色谱柱之间零死体积的连接器。在上述条件下,使用15cm×2mm内径的YGW(5μm)硅胶液相色谱柱和60m×0.25mm内径的OV - 101气相色谱柱,通过该系统对轻质柴油中的芳烃进行了分离和分析。分析结果表明,HPLC与CGC在线联用系统是分析复杂混合物中微量成分的可靠分析工具,尤其适用于那些在气相色谱分析前需要进行样品制备的成分。