High-Speed GC and GC/Time-of-Flight MS of Lemon and Lime Oil Samples

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Abstract
The high-speed GC separation and MS characterization of lime oil and lemon oil samples using programmable column selectivity and time-of-flight mass spectrometry is described. The volatile essential oils are separated on a series-coupled (tandem) column ensemble consisting of a polar trifluoropropylmethyl polysiloxane column and a nonpolar 5% phenyl dimethyl polysiloxane column. Both columns are 7 m long. A 50 °C/min linear temperature ramp from 50 to 200 °C is used, giving an analysis time of ∼2.5 min. A time-of-flight MS with time array detection and automated peak finding and characterization software was used to identify 50 components in lime oil samples and 25 components in lemon oil samples. Despite numerous cases of extensive peak overlap, spectral deconvolution software was very successful in the characterization of most overlapping peaks. For cases where a more complete chromatographic separation is desirable, the tandem column ensemble is operated in the first-column stop-flow mode to enhance the separation of selected overlapping clusters of peaks. A valve between the junction point of the tandem column ensemble and a source of carrier gas at the GC inlet pressure is opened for 2−5-s intervals to stop the flow of carrier gas in the first column. This is used to increase the separation of target component groups that overlap in the ensemble chromatogram without first-column stop-flow operation. This procedure is used to isolate the peak for limonene, the largest peak in the analytical-ion chromatogram of both the lime and lemon oil samples.