New Opportunities for Wine Analysis through SPME Arrow and GC-MS/MS

Significance of Topic

Gas chromatography–mass spectrometry (GC-MS) remains a cornerstone in wine analysis, enabling detailed profiling of aroma compounds and contaminants. Recent advances in solid-phase microextraction Arrow (SPME Arrow) improve sample throughput, sensitivity and robustness, addressing the challenges of small sample volumes and complex matrices typical of high-value aged wines.

Objectives and Study Overview

This study evaluates the performance of an automated SPME Arrow–GC-MS/MS workflow for two wine analysis applications: the quantification of mint-related volatile aroma compounds in aged red Bordeaux wines and the screening of pesticide residues. The goals include reducing sample volume, enhancing sensitivity, improving repeatability and assessing feasibility as an alternative to established extraction methods.

Methods and Instrumentation

Sample preparation is simplified to a 5 mL aliquot in headspace vials, with optional dilution to mitigate ethanol effects. Key methodological steps:

• SPME Arrow extraction in direct immersion or headspace mode, optimizing fiber coating (PDMS-DVB selected), extraction time, temperature and salt addition.
• Analysis by a Thermo Scientific TSQ 8000 Evo triple quadrupole GC-MS/MS coupled to a TriPlus RSH autosampler with automatic tool change.
• Data acquisition and quantitation using Chromeleon CDS software, with internal standards to improve repeatability.

Main Results and Discussion

The SPME Arrow approach demonstrated high linearity (r2 > 0.99 for most aroma compounds) and low limits of detection (sub-µg/L levels). Recovery rates for minty volatiles ranged from 80 % to 120 % across spiking levels, with repeatabilities (RSD) under 15 % when using internal standards. In pesticide residue screening, SPME Arrow in immersion produced higher peak areas than QuEChERS or SPE, with residual memory effects below 1 µg/L. Overall, the automated workflow yielded robust quantitation and minimal sample preparation bias.

Benefits and Practical Applications

The SPME Arrow–GC-MS/MS method offers:

• Reduced sample consumption, crucial for aged or rare wines.
• Full automation from extraction to detection, increasing laboratory throughput.
• Enhanced sensitivity and selectivity for trace aroma compounds and pesticide residues.
• Improved repeatability and reduced risk of co-elution through tandem MS detection.

Future Trends and Opportunities

Emerging directions include:

• Simultaneous analysis of haloanisoles and halophenols linked to cork taint at sub-sensory levels.
• Integration with high-resolution MS for non-target screening of wine contaminants.
• Expansion to other liquid food matrices where minimal sample volumes and high throughput are required.

Conclusion

The SPME Arrow–GC-MS/MS platform constitutes a versatile and efficient tool for advanced wine quality assessment, combining minimal sample handling, high automation and excellent analytical performance. It holds promise as a routine solution for volatile profiling and contaminant monitoring in enology.

Reference

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4. Picard M., Franc C., de Revel G., Marchand S. Anal. Chim. Acta 2018, 1001, 168–178.