Development of a routine analysis of 4-mercapto-4-methylpentan-2-one in wine by stable isotope dilution assay and mass tandem spectrometry

• We proposed a routine method to analyze the 4-methyl-4-mercaptopentan-2-one in wine.
• We developed the first method with sensitivity below the 4MMP perception threshold.
• We obtained an accurate method by using the stable isotope dilution assay approach.

The 4-mercapto-4-methylpentan-2-one (4MMP) is a key aroma compound in wines, especially in Sauvignon Blanc ones. Its accurate quantification is quite difficult due to its traces levels and its reactivity in wine conferred by the thiol function. In this paper, we proposed a new method for its quantification in wine without any sample preparation, based on automated derivatization procedure by methoximation and SIDA–SPME–GC–MS/MS analysis. The derivatization procedure was adapted from a previously published method in order to decrease the amount of reagents and the volume of wine (only 3 mL are required). The use of SPME and the detection conditions have also been optimized to reach the best sensitivity as possible. The method was then validated according to the International Organization of Vine and Wine recommendations and exhibited excellent performances. Indeed, this method allowed us to quantify the 4MMP in wine at traces levels (LOD = 0.19 ng L−1) with reproducible results (RSD < 15%) and a very good accuracy (recovery = 102%).

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