AS303: Analytical Workflows for Distilled Spirits Analysis


12th June 2023

Measurement of the volatile profiles of alcoholic beverages, such as Whisky, are important both for understanding the impact of processes on flavour characteristics and investigating counterfeit products. Compounds of interest may be present at extremely low levels, resulting in the requirement for highly sensitive and robust methods.

There are a number of techniques that can be employed for the analysis of flavours from liquid samples, many of which can be fully automated. For some spirits, a simple ‘dilute and shoot’ approach may be possible, but in order to meet the required limits of detection, some degree of enrichment is often required.

Automated liquid- liquid extraction, including Dispersive Liquid Liquid Micro Extraction (DiLLME) and headspace techniques such as Solid Phase Microextraction (SPME) or Dynamic Headspace (DHS) can provide the required degree of enrichment for this type of analysis.

The use of comprehensive 2- Dimensional GC (GCxGC) and fast scanning TOFMS instrumentation can also enhance the number of compounds detected and simplify data processing. Statistical data mining approaches can aid the identification of differences between samples.

This application note discusses the choice of sample preparation technique for distilled spirit analysis and offers examples of sample extraction and data analysis strategies. It clearly shows that the most suitable sample extraction technique will depend on the matrix and analytes of interest. Direct immersion (Stir Bar Sorptive Extraction (SBSE) can give increased response for the less volatile analytes, although may not extract the more polar compounds. DHS Fully Evaporative Technique (FET) and MultiVolatile Method (MVM), in general yield the broadest range of analytes. SPME is a good choice for obtaining a general profile of a sample, although can show some bias towards the most volatile components.


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