Multidimensional Gas Chromatography of Organosulfur Compounds in Coffee and Structure-Odor Analysis of 2-Methyltetrahydrothiophen-3-one.

Organosulfur compounds (OSCs) in coffee remain challenging to analyze by conventional gas chromatography (GC) due to their low concentrations amid coffee's complex matrix and susceptibility to chiral-odor influences. In this study, multidimensional GC (MDGC) methods were developed to profile OSCs in coffee. Conventional GC was compared to comprehensive GC (GC×GC) for untargeted OSC analysis in eight specialty coffees, and GC×GC was found to improve the fingerprinting of OSCs in coffee (50 vs 16 OSCs identified). Of the 50 OSCs, 2-methyltetrahydrothiophen-3-one (2-MTHT) was of high interest due to its chirality and known aroma contribution. Following that, a heart-cutting method for chiral GC (GC-GC) was developed, validated, and applied to the coffees. The mean enantiomer ratio of 2-MTHT was observed to be 1.56 (R/S) in brewed coffees. Overall, MDGC techniques allowed for more comprehensive analyses of coffee OSCs, from which (R)-2-MTHT was found to be the predominant enantiomer with the lower odor threshold.

Characterisation of catechins and their oxidised derivatives in Ceylon tea using multi-dimensional liquid chromatography and high-resolution mass spectrometry.

Tea is a complex food matrix comprising of many structurally diverse compounds, of which catechins and their oxidised derivatives are of particular interest due to their nutritional functionality. However, these catechins and derivatives exist in various isomeric forms with few or no pure standards available, rendering their analysis challenging. A method combining multi-dimensional liquid chromatography (MDLC) and high-resolution mass spectrometry (HRMS) was developed for the characterisation of these compounds using Ceylon tea as a model. Based on a Plackett-Burman (PB) design, flow rate and initial methanol percentage were identified as the most significant factors (p < 0.05) affecting chromatogram coverage and resolution (Rs) for comprehensive two-dimensional LC (LCxLC) and heart-cutting two-dimensional LC (LC-LC) respectively. Central composite design (CCD) was then applied using these parameters for method optimisation and to identify second-order relationships between screened parameters. The optimised LCxLC (flow rate: 2.18 mL/min and initial methanol percentage: 28.0%) and LC-LC (flow rate: 0.86 mL/min and initial methanol percentage for different cuts: A- 10.0%; B- 15.8%; and C- 18.7%) methods were applied to the analysis of Ceylon tea samples from seven regions of Sri Lanka and demonstrated an improved separation of co-eluting isomeric compounds. Finally, with the mass spectral information from HRMS, a total of 31 compounds (eight monomers, 17 dimers, five trimers and one tetramer) were detected and putatively identified in Ceylon tea.

Biovalorization of spent Konacha tea leaves via single-culture fermentation involving wine yeasts and lactic acid bacteria.

AIMS: The objective of this study was to explore the potential of fermentation as a biovalorization strategy for spent tea leaves (STL), a major agrifood waste generated from the tea extraction industry. Fermentation by wine yeasts or lactic acid bacteria (LAB) has shown promising results in previous studies across various substrates. METHODS AND RESULTS: Konacha (green tea) STL slurries were inoculated with single strains of wine yeasts or LAB respectively. After a 48-h fermentation, changes in selected nonvolatile and volatile compositions were evaluated. Fermentation by LAB increased organic acid content by 5- to 7-fold (except Lactobacillus fermentum) and modulated the composition of major tea catechins, whereas wine yeast fermentation resulted in a 30% increase in amino acid content. Strain-specific production of specific volatile compounds was also observed such as butanoic acid (L. fermentum), isoamyl acetate (Pichia kluyveri) and 4-ethylphenol (L. plantarum). CONCLUSIONS: Both volatile and nonvolatile compound compositions of Konacha STL were successfully modified via wine yeast and LAB fermentation. SIGNIFICANCE AND IMPACT OF STUDY: Our findings indicate that Konacha STL is a suitable medium for biovalorization by wine yeasts or LAB via the generation of commercially useful volatile and nonvolatile compounds. Future optimizations could further render fermentation an economically viable strategy for the upcycling of STL.

Recent advances in analytical strategies for coffee volatile studies: Opportunities and challenges.

Coffee has attracted significant research interest owing to its complex volatile composition and aroma, which imparts a pleasant sensorial experience that remains challenging to analyse and interpret. This review summarises analytical challenges associated with coffee's volatile and matrix complexity, and recent developments in instrumental techniques to resolve them. The benefits of state-of-the-art analytical techniques applied to coffee volatile analysis from experimental design to sample preparation, separation, detection, and data analysis are evaluated. Complementary method selection coupled with progressive experimental design and data analysis are vital to unravel the increasing comprehensiveness of coffee volatile datasets. Considering this, analytical workflows for conventional, targeted, and untargeted coffee volatile analyses are thus proposed considering the trends towards sorptive extraction, multidimensional gas chromatography, and high-resolution mass spectrometry. In conclusion, no single analytical method addresses coffee's complexity in its entirely, and volatile analysis must be tailored to the key objectives and concerns of the analyst.