Volatile Sulfur Compounds in Cheddar Cheese Determined by Headspace Solid-Phase Microextraction—Gas Chromatography—PFPD

Author(s):  
Michael C. Qian ◽  
Helen M. Burbank
Molecules ◽  
2019 ◽  
Vol 24 (18) ◽  
pp. 3320 ◽  
Author(s):  
Peter M. Davis ◽  
Michael C. Qian

The analysis of volatile sulfur compounds using headspace solid-phase microextraction (HS-SPME) is heavily influenced by matrix effects. The effects of a wine matrix, both non-volatile and volatile components (other than ethanol) were studied on the analysis of several common sulfur volatiles found in wine, including hydrogen sulfide (H2S), methanethiol (MeSH), dimethyl sulfide (DMS), dimethyl disulfide (DMDS), dimethyl trisulfide (DMTS), diethyl disulfide (DEDS), methyl thioacetate (MeSOAc), and ethyl thioacetate (EtSOAc). Varying levels of devolatilized wine and common wine volatiles (acids, esters, alcohols) were added to synthetic wine samples to act as matrices. Sulfur standards were added and analyzed using gas chromatography with pulsed-flame photometric detection (GC-PFPD). Five internal standards were used to find best representatives of each compound despite matrix effects. Sensitivity remained stable with the addition of devolatilized wine, while addition of volatile components decreased sensitivity. DMS was found to be best measured against EMS; DMDS and the thioacetates were best measured against DES; H2S, MeSH, DEDS, and DMTS were best measured against DIDS. The method was used to quantitate the volatile sulfur compounds in 21 wines with various ethanol contents and volatile profiles.


Molecules ◽  
2020 ◽  
Vol 25 (5) ◽  
pp. 1232
Author(s):  
Urszula Dziekońska-Kubczak ◽  
Katarzyna Pielech-Przybylska ◽  
Piotr Patelski ◽  
Maria Balcerek

Volatile sulfur compounds (VSCs) play an important role in the aroma profile of fermented beverages. However, because of their low concentration in samples, their analysis is difficult. The headspace solid-phase microextraction (HS–SPME) technique coupled with gas chromatography and mass spectrometry (GC–MS) is one of the methods successfully used to identify VSCs in wine and beer samples. However, this method encounters more obstacles when spirit beverages are analyzed, as the ethanol content of the matrix decreases the method sensitivity. In this work, different conditions applied during HS–SPME/GC–MS analysis, namely: ethanol concentration, salt addition, time and temperature of extraction, as well as fiber coating, were evaluated in regard to 19 sulfur compounds. The best results were obtained when 50/30 μm Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS) was used to preconcentrate the analytes from the sample at 35 °C for 30 min. The dilution of samples to 2.5% v/v ethanol and the addition of 20% w/v NaCl along with 1% EDTA significantly improves the sensitivity of extraction. The optimized method was applied to three fruit brandy samples (plum, pear, and apple) and quantification of VSCs was performed. A total of 10 compounds were identified in brandy samples and their concentration varied greatly depending on the raw material used from production. The highest concentration of identified VSCs was found in apple brandy (82 µg/L).


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