Fast GCXGC with short primary columns

摘要

A novel approach to comprehensive two-dimensional gas chromatography (GC x GC) separations is presented, which operates in a new region of the "GCxGC optimization pyramid". The technique relies on the use of short primary columns to decrease elution temperatures (T,) of analytes from the primary column, with a T, reduction of up to 50 degrees C illustrated. This in turn has implications that will expand the areas where GC x GC can be used, as decreased elution temperatures will allow GCxGC to be applied to mixtures of less volatile compounds or permit the use of less thermally stable stationary phases in the column ensemble. As well, it will allow GCxGC to be applied to thermally labile compounds through a reduction in elution temperature. With short primary columns, resolution and efficiency in the first dimension is sacrificed, but speed is gained; however, the second column in GC x GC provides additional resolution and separation of compounds of differing chemical properties. Thus, it is possible to recover some of the analytical separation power of the system to provide resolution of target analytes from sample impurities. As an example, a case study using short primary columns for the separation of natural pyrethrins, which degrade above 200 degrees C, is described. Even with the sacrifices of overall separation power that are made, there is still sufficient resolution available to separate the six natural pyrethrins from each other and the complex chrysanthemum extract matrix. The use of cold-on-column injection, a short primary column, and a high carrier gas flow rate allow the pyrethrins to be eluted below 200 degrees C, with separation in 17 min and complete resolution from sample matrix.