Optimized use of a 50 μm 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 50 mu m ID secondary column, in a comprehensive two-dimensional gas chromatography-quadrupole mass spectrometry (GC x GC-qMS) system. The analytical aim was achieved by exploiting a split-flow GC x GC approach, and a rapid-scanning qMS instrument. The stationary phase combination consisted of an apolar (silphenylene polymer) 30 m x 0.25 mm ID column, linked by means of a Y-union, to an MS-connected 1 m x 0.05 mm ID polar one[poly(ethyleneglycol)], and to a 0.20 m x 0.05 mm ID uncoated capillary segment; the latter was connected to a manually operated split-valve. It will be herein demonstrated that the split-flow GC x GC approach, successfully employed in previous H-2-based, flame ionization detection experiments, provides equally satisfactory results using mass spectrometric detection and helium as carrier gas. An optimized split-flow GC x 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 50 mu m ID secondary column in a conventional GC x GC-MS instrument. On the contrary, the use a 50 mu m 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. (C) 2010 Elsevier B.V. All rights reserved.