Bordajandi Luisa R, Korytár Peter, de Boer Jacob, González María José
Dept of Instrumental Analysis and Environmental Chemistry, Institute of Organic Chemistry, CSIC, 28006 Madrid, Spain.
J Sep Sci. 2005 Feb;28(2):163-71. doi: 10.1002/jssc.200401868.
Three commercially available chiral capillary columns, Chirasil-Dex, BGB-176SE, and BGB-172, have been evaluated for the separation into enantiomers of the 19 chiral polychlorinated biphenyls (PCB) congeners stable at room temperature. The enantiomers of 15 chiral PCBs were, at least to some extent, separated using these beta-cyclodextrin based columns. Multidimensional techniques, such as heart-cut multi-dimensional gas chromatography (heart-cut MDGC) and comprehensive two-dimensional gas chromatography (GC x GC), were investigated for their ability to solve coelution problems with other PCBs present in commercial mixtures and real-life samples. Heart-cut MDGC improved the separation as compared to one-dimensional GC, and enantiomeric fractions of the investigated chiral PCBs could be determined free from interferences. However, limitations on the number of target compounds that can be transferred to the second column in a single run and, therefore, the time consumption, have led to the evaluation of GC x GC as an alternative for this type of analysis. With GC x GC, two column set-ups were tested, both having a chiral column as first-dimension column, and two different polar stationary phase columns in the second dimension. On using both column combinations, congeners 84, 91, 95, 132, 135, 136, 149, 174, and 176 could be determined free from coelutions with other PCBs. Results on the application of heart-cut MDGC to food samples such as milk and cheese are given, as well as the first results on the application of GC x GC to this type of samples.
已对三种市售手性毛细管柱Chirasil-Dex、BGB-176SE和BGB-172进行了评估,以将19种在室温下稳定的手性多氯联苯(PCB)同系物拆分为对映体。使用这些基于β-环糊精的色谱柱,至少在一定程度上拆分了15种手性多氯联苯的对映体。研究了多维技术,如中心切割多维气相色谱法(中心切割MDGC)和全二维气相色谱法(GC×GC),以解决其与商业混合物和实际样品中存在的其他多氯联苯共洗脱问题的能力。与一维气相色谱相比,中心切割MDGC改善了分离效果,并且可以在不受干扰的情况下测定所研究手性多氯联苯的对映体分数。然而,单次运行中可转移到第二根色谱柱的目标化合物数量有限,因此耗时较长,这促使人们对GC×GC作为此类分析的替代方法进行评估。对于GC×GC,测试了两种柱设置,两种设置均以手性柱作为第一维色谱柱,在第二维使用两种不同的极性固定相色谱柱。使用这两种柱组合时,可以在不存在与其他多氯联苯共洗脱的情况下测定同系物84、91、95、132、135、136、149、174和176。给出了中心切割MDGC应用于牛奶和奶酪等食品样品的结果,以及GC×GC应用于此类样品的初步结果。