The Determination of 2,4,6-Trichloroanisole in Wine using Headspace Trap with GC/MS

Importance of the Topic

The presence of 2,4,6-trichloroanisole (TCA) even at parts-per-trillion levels can impart an undesirable cork taint to wine, affecting aroma and flavor. Accurate detection at these ultra-trace levels is essential for quality control in oenology and consumer satisfaction.

Objectives and Overview

This study evaluates a headspace trapping technique combined with gas chromatography–mass spectrometry (GC–MS) for sensitive, precise quantification of TCA in wine bottles sealed with cork. The aim is to achieve low detection limits while maintaining high throughput and reproducibility.

Methodology and Instrumentation

Sample Preparation:

• Ten grams of commercial white wine placed in a 22 mL headspace vial sealed with baked silicone/PTFE septa.
• Spiking with a 100 ppb TCA standard to prepare calibration at 10 ppt and 100 ppt.

Instrumentation:

• TurboMatrix HS-40 Headspace Trap equipped with Carbopack Y sorbent, operated at 40 °C (trap low) and 280 °C (trap high), needle temperature 75 °C.
• PerkinElmer Clarus 500 GC with Elite-5MS column (30 m × 0.25 mm, 0.25 µm), split/splitless injector at 150 °C, oven program from 50 °C to 240 °C.
• Clarus 500 MS using single-ion full-scan (SIFI) acquisition; monitoring m/z 210 and 195 with electron ionization at 70 eV.

Main Results and Discussion

The headspace trap approach achieved a 100-fold sensitivity enhancement over static headspace, reaching detection at the 10 ppt level. Chromatographic separation and selected ion recording (m/z 210, 195) allowed clear identification of TCA despite matrix interferences. Library spectrum matching confirmed analyte identity. Throughput was demonstrated at 50–75 analyses per day with automated sample loading.

Benefits and Practical Applications

The described method provides:

• Ultra-trace detection limits compatible with sensory thresholds.
• Automated workflow requiring minimal sample handling.
• High throughput suitable for routine quality control in wineries.

Future Trends and Potential Applications

Continued development may include:

• Extension of headspace trap GC–MS to other trace wine contaminants and flavor compounds.
• Integration with chemometric calibration models for rapid screening.
• Application of advanced sorbents and temperature programming to improve selectivity and sensitivity.

Conclusion

The TurboMatrix HS-40 headspace trap coupled with PerkinElmer Clarus 500 GC–MS meets stringent requirements for TCA analysis in wine, offering low-ppt detection, automation, and robust performance for routine quality control.

References

1. For Quality Control of Natural Corks, www.corkqc.com/SPMEFAQ.htm.
2. M.P. Marti et al Fast Screening Method for Determining 2,4,6-Trichloroanisole in Wines using Headspace-MS and Multivariate Calibration, Anal Bioanal Chem, 2003, 376, pp 497–501.