Volatile Sulphur Compounds in Wine Distillates by Stir Bar Sorptive Extraction-Gas Chromatography-Mass Spectrometry

Abstract

A Stir Bar Sorptive Extraction-Gas Chromatography-Mass Spectrometry (SBSEGC-MS) method has been optimized and validated for the determination of eight volatile sulphur compounds in wine distillates: diethyl sulphide (DES), dimethyl disulphide (DMDS), diethyl disulphide (DEDS), 2-thiophenecarboxaldehyde (TC), dibutyl sulphide (DBS), dipropyl disulphide (DPDS), dipropyl sulphide (DPS), and dimethyl trisulphide (DMTS). After optimization by 24 factorial design, the SBSE-GC-MS extraction conditions were as follows: a polydimethylsiloxane twister (10 mm × 0.5 mm), 35 ◦C as the extraction temperature, 10 mL as the sample volume, 7% (v/v) as the alcoholic grade, 47 min as the extraction time, 10% (w/v) of NaCl, and 1% (w/v) of EDTA (ethylenediaminetetraacetic acid). Under optimal conditions, adequate analytical figures of merit were obtained for eight of the ten compounds initially considered, with low quantification and detection limits and relative standard deviations for inter-twister and inter-day repeatability values ranging from 7.5 to 21.8% and from 7.2 to 27.5%, respectively. The methodology was applied to 34 wine distillates (continuous column distillation and distillation in pot still) elaborated for the production of Brandy de Jerez: 15 aged distillates aged for different periods of time in American oak wood and 19 non-aged distillates. The most significant volatile sulphur compounds were DBS, DMDS, and DPS. The Cluster Analysis (CA) on the volatile sulphur compounds grouped the samples according to the use of sulphur dioxide. In general, lower amounts of volatile sulphur compounds were found in the aged samples, although the high standard deviations obtained highlight that their contents depend on multiple factors related to the elaboration process.