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 30 m×0.25 mm id×0.25 μm dfcapillary linked, viaa T‐union, to a secondary polar 1.0 m×0.05 mm id×0.05 μm dfcapillary and to a 0.10 m×0.05 mm id×0.05 μm dfuncoated column segment. The GC×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 first‐dimension effluent to waste and enabled the generation of optimum gas velocities in both dimensions, namely circa20 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 time+interscan time: 40 ms), and with a normal GC mass range (m/z40–360). Chromatography bands at the second‐dimension outlet were never less than 360 ms wide (6σ), enabling the acquisition of at least 10 spectra/peak.