The development of the MVM (Multi-Volatile Method) in the whisky matrix

Significance of the topic

Comprehensive analysis of volatile compounds in whisky is essential for quality control, flavor profiling and authentication. Traditional single‐trap dynamic headspace techniques often fail to recover highly volatile analytes, leading to incomplete aroma characterization. The Multi‐Volatile Method (MVM) offers a novel approach to expand the detectable range of volatiles in a single chromatographic run, improving data richness for sensory, research and industrial applications.

Objectives and Overview

This application note describes the adaptation of GERSTEL’s Multi‐Volatile Method to a whisky matrix using two sorbent traps instead of three. The goals were to optimize extraction parameters, assess reproducibility, compare performance against a conventional single‐trap DHS, and demonstrate enhanced recovery of key whisky volatiles.

Methodology

MVM employs sequential dynamic headspace extractions on the same sample vial, followed by staged thermal desorption into a cooled inlet system. Two traps were used:

• Carboxen 1000/Carbopack B+X (55 °C incubation; 10 mL headspace draw; small dry phase)
• Tenax TA (80 °C incubation; 750 mL headspace draw; extended dry phase)

The desorption sequence started with Tenax TA at CIS 10 °C, then Carboxen/Carbopack at CIS –50 °C. Both traps were ramped in the Thermal Desorption Unit (30 °C to 300 °C splitless) and focused in the CIS before transfer to the DB-WAX column. GC-MS conditions included an Agilent 7890A GC with single quadrupole MS in full scan mode.

Instrumental Setup

• Agilent GC 7890A with QQQ MS detector (full scan)
• Gerstel MPS 2 dual‐head autosampler
• Thermal Desorption Unit / Cooled Inlet System (TDU/CIS)
• DB-WAX capillary column
• Agilent MSD ChemStation and Gerstel Maestro software

Main Results and Discussion

Reproducibility was evaluated with two internal standards (butyl acrylate for Carboxen/Carbopack and benzyl d-5 alcohol for Tenax). RSD values for selected whisky volatiles ranged from 2.3 % to 8.2 %, indicating robust performance. Overlayed chromatograms of five replicates showed consistent peak intensities and retention times. Comparative experiments revealed that MVM provided higher signal intensities and more complete recovery of both mid‐ and highly volatile compounds than a single Tenax TA extraction.

Benefits and Practical Applications

• Extended volatility range in a single analysis without multiple injections
• Improved detection of highly volatile analytes (e.g., acetaldehyde, light hydrocarbons)
• Better peak shapes and separation due to reverse desorption order
• Enhanced throughput for flavor profiling, authenticity testing and QA/QC

Future Trends and Applications

Further improvements may include integrating a third trap for ultra-light volatiles, exploring alternative sorbent combinations such as Shincarbon X for trace aldehydes, and coupling MVM with high-resolution MS or real-time data analytics. The methodology could also be extended to other food and beverage matrices, environmental monitoring and forensic investigations.

Conclusion

The adapted MVM using two sorbent traps enables reliable, reproducible and comprehensive volatile profiling in whisky. By combining sequential headspace extractions with differential desorption, the method overcomes limitations of single‐trap approaches and streamlines aroma analysis for research and industrial laboratories.

References

• N. Ochiai, J. Tsunokawa, K. Sasamoto, A. Hoffmann. Multi‐volatile method for aroma analysis using sequential dynamic headspace sampling with an application to brewed coffee. J. Chromatogr. A 1371 (2014) 65–73.