Unique VUV absorbance spectra not only enable unambiguous compound identification, and allows GC run times to be deliberately shortened. VUV detectors operate at ambient pressure and are thus not flow rate limited. GC run times can be reduced by increasing the GC column flow and oven temperature program rates.
Flow rate-enhanced chromatographic compression utilizes VUV spectral deconvolution to resolve any co-elution that may result from shortening GC runtimes. VUV absorption is additive, meaning that overlapping peaks give a spectrum that corresponds to the sum absorbance of each compound. The individual contribution of each analyte can be determined if the VUV spectra for co-eluting compounds are stored in the VUV library. The ability to differentiate coeluting analyte spectra and use them to deconvolve the overlapping signals is demonstrated in Figure 4. The individual spectra of terpenes limonene and p-Cymene are shown in Panel A along with the summed absorbance of the selected retention time window (blue region in Panel B) and the fit with VUV library spectra.  The R >0.999 fit result confirms their identities, and enables the deconvolution of these and other terpenes analyzed by GC-VUV as featured in Panel B.
Testing for the presence of residual solvents in Active Pharmaceutical Ingredients (APIs) is critical for patient safety and commonly follows United States Pharmacopeia (USP) Method <467> guidelines, or more broadly, International Council for Harmonization (ICH) Guideline Q3C(R6). The gas chromatography (GC) runtime suggested by USP Method 467 is approximately 60 min. A generic method for residual solvent analysis by GC-MS describes conditions that include a runtime of approximately 30 minutes. A GC-VUV and static headspace method was developed using a chromatographic compression strategy that resulted in a GC runtime of 8 minutes. The GC-VUV method uses a flow rate of 4 mL/min and an oven ramp of 35 °C (held for 1 min), followed by an increase to 245 °C at a rate of 30 °C/min.
Figure 5 compares the results when the general conditions of the GC-MS method were followed against the GC-VUV method run with Class 2 residual solvents. Tetralin eluted at approximately 35 minutes using the GC-MS method conditions, whereas the analyte had a retention time of less than 7 minutes when the GC-VUV method was applied. The co-elution of m- and p-xylene occurred in both GC-MS and GC-VUV method runs. VUV software matched the analyte absorbance of both isomers with VUV library spectra (Figure 2) to deconvolve the overlapping signals as displayed in Figure 6. Goodness of fit information ensures that the correct compound assignment takes place during the post-run data analysis.
The flow rate-enhanced chromatographic compression strategy has been applied to a diverse set of applications since the development of the GC-VUV method for residual solvents analysis. The fast GC-VUV approach reduced GC runtimes for terpene analysis from 30 minutes to 9 minutes (the deconvolution of monoterpene isomers is shown in Figure 4). It has also been demonstrated that GC runtimes as short as 14 minutes can be used for PIONA compound analysis of gasoline samples. Typical GC separation times range between 1 – 2 hours using alternative methods.