GC-TOF MS wine aroma profiling with variable energy ionization
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This presentation was delivered by Dr Laura McGregor of Markes International and Dr Luca Calamai of the University of Florence at the 38th ISCC & 11th GCxGC, Riva del Garda, Italy in May 2014. Also included is a case study on 'Enhanced screening of environmental pollutants in complex matrices by GC×GC–TOF MS'.
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GC-TOF MS wine aroma profiling with variable energy ionization
- 1. Enhanced aroma profiling of wine by GC–TOF MS with variable-energy ionisation 38th ISCC & 11th GCxGC, Riva Del Garda Markes International – vendor seminar Laura McGregor1, Luca Calamai2,3 Steve Smith1 and Nick Bukowski1 1. Markes International, Gwaun Elai Medi-Science Campus, Llantrisant, RCT, UK 2. Centro Interdipartimentale di Servizi di Spettrometria di Massa, Via U. Shiff 6, 50016 Sesto Fiorentino , (FIrenze) 3. Dip. Scienze delle Prod. Agroalimentari e dell’ambiente (DISPAA), Univ. degli studi di Firenze, Piazzale Cascine 28, 50144 Firenze
- 2. Wine aroma is a complex combination of a wide number of simple sensory perceptions What gives wine it’s characteristic aroma is... Source: zinfandel.org … A combination of many different volatile compounds typical of each wine Off odours
- 3. Approaches for characterising wine aroma Sensory vs. Analytical Source: www.arcus.no sensitivity Major Drawbacks Major Advantages sensitivityreproducibility Uses sensory descriptors and their intensity as assessed by Use compounds identification and quantification by reproducibility Panel test (5-30 members) HS–(GC)–MS analysis
- 4. Analytical approach for studying wine aroma Headspace–SPME sampling 15 min 1 mL wine 4 mL water 2 g NaCl 40 uL ISTD mix 60 ºC DVB/carboxen/PDMS fiber (50/30 µm). GC–TOF MS BenchTOF-Select: Data rate: 4 Hz Mass range: 30–450 amu Ion source: 200 ºC Transfer line: 260 ºC Ionisation energy: variable GC Oven: 40 ºC for 1.0 min, 2 ºC/min to 60 ºC 3 ºC/min to 150 ºC 10 ºC/min to 200 ºC 25 ºC/min to 250 ºC (hold 10 min). Column: HP-Innowax (50 m ×200 µm ×0.4 µm) Injection:Splitless, 260 ºC.
- 5. Quantitative approach: Calibration Standard mix • The calibration standard mix spanned a wide range of target compounds prepared in same way as for wine aroma profiling (SPME) but using a 12% ethanol solution containing 0.5% tararic acid as a wine mimic matrix instead of 1mL of wine • Target compounds from 5 chemical classes: – Esters – Lactones – Aldehydes & Ketones – Alcohols & Terpene alcohols – Acids • Internal Standard compounds: two deuterium-labelled compounds or surrogate absent in samples for each class
- 6. Results Calibration standard with wine mimic matrix Ethyl acetate Isoamyl acetate 2-methyl-1- propanol Isoamyl alcohol Ethyl hexanoate Hexyl acetate Hexanol Ethyl octanoate Benzaldehyde Decanoic acid Ethyl decanoate Octanoic acid
- 7. The full presentation can be downloaded from the Markes website http://www.markes.com/Resources/Scientific- publications/Conference-presentations.aspx
- 8. Conclusions • Low energy ionisation aids identification and extends LoDs • Low energy ionisation aids identification and extends LoDs • 70 eV and 14 eV give comparable quantitative results • GC×GC allows additional compounds to be identified – Off-odours – Fungicides – Compounds at ultra-trace level
- 9. Case study 2: Enhanced screening of environmental pollutants in complex matrices by GC××××GC–TOF MS A collaboration with…
- 10. Water Framework Directive (WFD) • Lower detection limits • New monitoring methods and analytical techniques are now necessary • Focus is on “priority” substances, but what about those of emerging concern?
- 11. Conclusions & Further Work • Promising start to the project; Select-eV adds an extra dimension of information • Quantitation of POPs required • Compare local drinking water/pollution levels with prosthesis extracts
- 12. Acknowledgements • Anthony Gravell (NRW), Ian Allan (NIVA) and Graham Mills (Portsmouth Uni) • N. Bukowski, G. Davies, D. Barden and S. Smith, Markes International • Luca Calamai, University of Florence
- 13. The full presentation can be downloaded from the Markes website http://www.markes.com/Resources/Scientific- publications/Conference-presentations.aspx