GC×GC-TOFMS/FID setup for qualitative and quantitative fragrance analysis (Joe Binkley, MDCW 2023)

🎤 Presenter: Elizabeth Humston-Fulmer¹, Joe Binkley¹, Nick Jones¹, Sebastiano Panto², Lena Dubois² (¹LECO Corporation, Saint Joseph, MI, USA. ²LECO European Applications and Technical Centre, Berlin, Germany)

Abstract

Fragrances are composed of tens or hundreds of ingredients, selected from a palate of thousands. The identification and quantification of individual species in a fragrance is challenging, and using numerous standards is not practically efficient. Therefore, a dual workflow is commonly employed using MS for identification and FID, with effective carbon number correction factors applied, for quantification. Additionally, due to the complexity of these samples, two analyses are often required to isolate the individual compounds; one using polar and another using a non-polar GC separation.

Here, we demonstrate a possible improvement to this workflow, using a prototype GCxGC-TOFMS/FID instrument. GCxGC provides enhanced chromatographic separation of individual analytes, removing the requirement for two separate 1D assays. Applying dual detection, using MS and FID, enables both identification from MS data and quantification via the FID. Quantification accuracy can be affected with many fixed or EPC splitters due to variation of the split ratio across the analytical run. The prototype instrument used in this study, uses a reverse fill flush modulator, allowing total transfer of the primary effluent to the secondary column, and a controlled splitter that maintains a consistent split ratio between the MS and FID. These characteristics help to ensure that biases are not introduced from changing split ratios over the course of the chromatographic separation, which could skew quantification results. Novel algorithms that align the MS and FID peaks facilitated data interpretation. Various fragrances were analyzed, with reliable analyte identifications and quantifications demonstrated from single injections.