Evaluation of comprehensive two-dimensional gas chromatography coupled to rapid scanning quadrupole mass spectrometry for quantitative analysis

Comprehensive two-dimensional gas chromatography (GC × GC) is a powerful technique that provides
excellent separation and identification of analytes in highly complex samples with considerable increase
in GC peak capacities. However, since second dimension analyses are very fast, detectors with a rapid
acquisition rate are required. Over the last years, quite a number of studies have discussed the potential
and limitations of the combination GC × GC with a variety of quadrupole mass spectrometers. The
present research focuses on the evaluation of qMS effectiveness at a 10,000-amu/s scan speed and 20-Hz
scan frequency for the identification (full scan mode acquisition-TIC) and quantification (extracted ion
chromatogram) of target pesticide residues in tomato samples. The following MS parameters have been
evaluated: number of data points per peak, mass spectrum quality, peak skewing, and sensitivity. The
validated proposed GC × GC/qMS method presented satisfactory results in terms of repeatability (coefficient
of variation lower than 15%), accuracy (84–117%), and linearity (ranging from 25 to 500 ng/g), while
significant enhancement in sensitivity was observed (a factor of around 10) under scan conditions.