Analysis of volatile thiols in alcoholic beverages by simultaneous derivatization/extraction and liquid chromatography-high resolution mass spectrometry

Abstract

A simultaneous derivatization/extraction method followed by liquid chromatography electrospray-high resolution mass spectrometry for the determination of volatile thiols in hydroalcoholic matrixes was optimized and used to identify and quantify volatile thiols in wine and beer samples. The method was evaluated in terms of sensitivity, precision, accuracy and selectivity. The experimental LOQs of eleven thiols tested ranged between 0.01 ng/L and 10 ng/L. Intra-day relative standard deviation (RSD) was in general lower than 10% and inter-day RSD ranged between 10% and 30%. Recovery in the model and real matrixes ranged from 45% to 129%. The method was then applied for the analysis of four white wines and six beers. Five out of the eleven reference thiols were identified and quantified in the samples analysed. The non-target approach, carried out by monitoring the diagnostic ion at m/z 275.9922 [C13H10ONSe]+ in the fragmentation spectrum, allowed detecting, in the same samples, fourteen non-target thiols.