Effective analysis of rotundone at below-threshold levels in red and white wines using solid-phase microextraction gas chromatography/tandem mass spectrometry

Rotundone is an oxygenated sesquiterpene belonging to the family of guaianes, giving the ‘peppery’ aroma to white and black pepper and to red wines. Here we describe a novel, convenient protocol for the synthesis of rotundone, starting from a commercially available compound and requiring only two re...

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Bibliographic Details
Published in:Rapid communications in mass spectrometry 2011-02, Vol.25 (4), p.483-488
Main Authors: Mattivi, F., Caputi, L., Carlin, S., Lanza, T., Minozzi, M., Nanni, D., Valenti, L., Vrhovsek, U.
Format: Article
Language:English
Subjects:
Aroma
Food Analysis - methods
Gas Chromatography-Mass Spectrometry - methods
Mass spectrometry
Monitoring
Oxygenated
Piper nigrum
Repeatability
Reproducibility
Reproducibility of Results
Sensitivity and Specificity
Sesquiterpenes - analysis
Sesquiterpenes - chemistry
Solid Phase Microextraction - methods
Tandem Mass Spectrometry
Vitaceae
Wine - analysis
Wines
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Description
Summary:Rotundone is an oxygenated sesquiterpene belonging to the family of guaianes, giving the ‘peppery’ aroma to white and black pepper and to red wines. Here we describe a novel, convenient protocol for the synthesis of rotundone, starting from a commercially available compound and requiring only two reaction steps, and an improved, faster method of GC separation (30 min) with selective quantisation of rotundone using tandem mass spectrometry in multiple reaction monitoring (MRM) mode with d5‐rotundone as internal standard. With limits of detection (LODs) of 1.5 ng/L in white wine and 2.0 ng/L in red wine, intraday repeatability CV values of 6% and 5% at 50 ng/L and 500 ng/L and interday repeatability CV values of 13% and 6% at 50 ng/L and 500 ng/L, respectively, the improved protocol provides the desired sensitivity and selectivity for routine analysis of rotundone in both white and red wines. Initial application of this method highlighted the presence of unexpectedly high concentrations of rotundone, thus explaining the origin of the distinctive peppery aroma in Schioppettino and Vespolina red wines and in Gruener Veltliner white wines. Copyright © 2011 John Wiley & Sons, Ltd.
ISSN:0951-4198
1097-0231
1097-0231
DOI:10.1002/rcm.4881