Solid phase extraction in combination with comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry for the detailed investigation of volatiles in South African red wines

Comprehensive two-dimensional gas chromatography in combination with time-of-flight mass spectrometry (GC × GC–TOFMS) has been applied for the analysis of volatile compounds in three young South African red wines. In spite of the significant benefits offered by GC × GC–TOFMS for the separation and identification of volatiles in such a complex matrix, previous results utilizing headspace solid phase micro extraction (HS-SPME) demonstrated certain limitations. These were primarily associated with the choice of sample preparation technique, which failed to extract some influential semi-volatile wine constituents. Therefore, in the current report, we utilized solid phase extraction (SPE) in combination with GC × GC–TOFMS for the detailed investigation of particularly low-level semi-volatiles in South African wine. 214 compounds previously reported in grapes and related beverages were tentatively identified based on mass spectral data and retention indices, while 62 additional compounds were positively identified using authentic standards. The method proved particularly beneficial for the analysis of terpenes, lactones and volatile phenols, and allowed us to report the presence of numerous volatile compounds for the first time in Pinotage wines.

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• A new SPE–GC × GC–TOFMS method for the analysis of wine volatiles is described.
• A detailed comparison with HS-SPME–GC × GC–TOFMS is presented.
• SPE–GC × GC–TOFMS beneficial for terpenes, volatile phenols and lactones.
• Identification by TOFMS is improved by removal of most polar volatiles during SPE.
• 276 compounds were identified, many for the first time in Pinotage wines.