Optimized use of a 50μm ID secondary column in comprehensive two-dimensional gas chromatography-mass spectrometry

The objective of the present research is directed towards the optimized use of a 50μm ID secondary column, in a comprehensive two-dimensional gas chromatography-quadrupole mass spectrometry (GC×GC-qMS) system. The analytical aim was achieved by exploiting a split-flow GC×GC approach, and a rapid-scanning qMS instrument. The stationary phase combination consisted of an apolar (silphenylene polymer) 30m×0.25mm ID column, linked by means of a Y-union, to an MS-connected 1m×0.05mm ID polar one [poly(ethyleneglycol)], and to a 0.20m×0.05mm ID uncoated capillary segment; the latter was connected to a manually operated split-valve. It will be herein demonstrated that the split-flow GC×GC approach, successfully employed in previous H2-based, flame ionization detection experiments, provides equally satisfactory results using mass spectrometric detection and helium as carrier gas. An optimized split-flow GC×GC-qMS method was developed and exploited for the analysis of a perfume sample. The results attained were compared with those observed using the same analytical column combination, but with no flow-splitting. It was found that it is not convenient to employ a 50μm ID secondary column in a conventional GC×GC-MS instrument. On the contrary, the use a 50μm ID secondary column, in a split-flow, twin-oven system, provided a good performance. A recently developed comprehensive chromatography software was used for data processing. © 2010 Elsevier B.V.