François Isabelle, Pereira Alberto dos Santos, Lynen Frédéric, Sandra Pat
Department of Organic Chemistry, Ghent University, Krijgslaan, Ghent, Belgium.
J Sep Sci. 2008 Oct;31(19):3473-8. doi: 10.1002/jssc.200800267.
The design of a new interface to hyphen high efficiency supercritical fluid chromatography (SFC) and fast RPLC in a comprehensive configuration is described. SFC x RPLC is a viable alternative to normal phase (NP) LC x RPLC and is characterized by high orthogonality. Compared to NPLC x RPLC an additional advantage is the expansion of supercritical carbon dioxide (CO(2)) when exposed to atmospheric pressure leading to fractions consisting of solvents that are miscible with the second dimension RPLC mobile phase. The interface consists of a two-position/ten-port switching valve equipped with two packed octadecyl silica (C(18)) loops for effective trapping and focusing of the analytes after elution from the SFC dimension. The addition of a water make-up flow to the SFC effluent prior to entering the loops is of fundamental importance to efficiently focus the solutes on the C(18) material and to reduce interferences of expanded CO(2) gas on the second dimension separation. The features of the system are illustrated with the analysis of a lemon oil sample.
描述了一种新型接口的设计，该接口用于将高效超临界流体色谱法（SFC）与快速反相液相色谱法（RPLC）以全二维配置联用。SFC×RPLC是正相液相色谱法（NP）×RPLC的一种可行替代方法，其特点是具有高正交性。与NP×RPLC相比，另一个优点是超临界二氧化碳（CO₂）在暴露于大气压时会膨胀，从而导致馏分由与二维RPLC流动相混溶的溶剂组成。该接口由一个两位十通切换阀组成，该阀配备有两个填充十八烷基硅胶（C₁₈）的定量环，用于在从SFC维度洗脱后有效捕集和聚焦分析物。在进入定量环之前向SFC流出物中添加补水流量对于将溶质有效地聚焦在C₁₈材料上并减少膨胀的CO₂气体对二维分离的干扰至关重要。通过对柠檬油样品的分析说明了该系统的特点。
