Accurate quadrupole MS peak reconstruction in optimized gas-flow comprehensive two-dimensional gas chromatography

In the present research, a split-flow comprehensive 2-D GC-quadrupole MS (qMS) method was developed using: a primary apolar 30m x 0.25mm id x 0.25 mm df capillary linked, via a T-union, to a secondary polar 1.0m x 0.05mm id x 0.05 mm df capillary and to a 0.10m x 0.05mm id x 0.05 mm df uncoated column segment. The GC x GC-qMS instrument was equipped with two GC ovens and a loop-type modulator. The polar column was connected to the MS, whereas the uncoated column directed most of the firstdimension effluent to waste and enabled the generation of optimum gas velocities in both dimensions, namely circa 20 and 80 cm/s in the first and second dimensions, respectively. The rapid-scanning qMS was operated at a scan speed of 10 000 amu/s, a 25-Hz data acquisition frequency (scan time1interscan time: 40 ms), and with a normal GC mass range (m/z 40-360). Chromatography bands at the second-dimension outlet were never less than 360 ms wide (6s), enabling the acquisition of at least 10 spectra/peak. © 2010 Wiley-VCH Verlag GmbH & Co. KGaA.