Determination of 2,4,6 Trichloroanisole in cork and wine with HS-SPME/GCMS - standard - fast

Importance of TCA Analysis

The presence of 2,4,6-trichloroanisole in cork stoppers and wine poses a significant quality risk due to its musty off-flavor detectable at low parts per trillion levels. Reliable and sensitive detection of this compound is essential for cork production quality control and for safeguarding wine sensory properties.

Objectives and Study Overview

This application note describes the development and validation of a fast headspace solid phase microextraction combined with gas chromatography mass spectrometry method to quantify 2,4,6-trichloroanisole in cork and wine samples. The goals included optimizing enrichment, achieving low detection limits, and demonstrating applicability to real-world matrices.

Methodology

Cork stoppers were extracted by immersion in 12 % ethanol water at room temperature for 24 h. An aliquot of the extract was salted with sodium chloride and spiked with deuterated TCA as internal standard. Headspace SPME was performed using a polydimethylsiloxane fiber at 50 °C for 30 min, followed by thermal desorption at 220 °C for 2 min. GCMS analysis used splitless injection with a high-pressure pulse, a short RTX-5 column (25 m × 0.25 mm × 0.25 µm), temperature programming from 50 °C to 260 °C, and selected ion monitoring of m/z 195 for TCA and m/z 215 for the internal standard.

Used Instrumentation

• Gas Chromatograph-Mass Spectrometer: Shimadzu GCMS-QP2010
• Autosampler: Shimadzu AOC-5000 with incubator for 20 mL headspace vials
• SPME Fiber: Polydimethylsiloxane (PDMS)
• Chromatographic Column: RTX-5, 25 m length, 0.25 mm I.D., 0.25 µm film

Main Results and Discussion

The method exhibited excellent linearity over 0.54 to 53.8 ppt TCA with a correlation coefficient of 0.99994. The quantitation limit was determined at approximately 0.7 ppt. Analysis of a cork sample yielded 6 ppt TCA, and a red wine spiked at 5 ppt produced a clearly defined peak in full scan mode. Fast GCMS with a narrow-bore column and optimized carrier gas velocity delivered sharp peaks (0.6 s width) and preserved sensitivity.

Benefits and Practical Applications

• Low-level detection of TCA for quality assurance of cork production and wine bottling
• Automated, high-throughput workflow suitable for routine laboratory screening
• Fast analysis times enabled by rapid temperature ramps and optimized carrier gas flow

Future Trends and Opportunities

Advances may include further miniaturization of extraction fibers, integration of high-resolution mass analyzers, and fully automated workflows. Coupling accelerated GCMS methods with data-driven quality control systems will enhance screening efficiency for trace off-flavor compounds.

Conclusion

This fast HS-SPME/GCMS method provides a robust, sensitive, and rapid approach for quantifying 2,4,6-trichloroanisole at sub-ppt levels in cork and wine. Its high linearity, low detection limit, and adaptability to routine analysis make it a valuable tool for ensuring product quality and preventing taint.

Reference

• [1] Shimadzu Application Book Chromatography Vol 2 Fast GC&GCMS by L Mondello and H U Baier