This work studies the microwave-assisted extraction conditions for recovery of polysaccharides from spent coffee grounds, including their effect on arabinogalactans and galactomannans polymerization and branching structural features. Temperature (140, 170, and 200 °C) has the most significant impact on total extracted mass (ηtotal soluble solids) and sugars yield (ηsugars), arabinogalactans (ηAG) and galactomannans (ηGM), and polysaccharide mass ratio (ηAG/ηGM). Time (2, 5, and 10 min) and alkali (diluted 0.1 M NaOH) treatments have less influence. Alkali treatment and shorter time (2 min) provided a protective effect against polysaccharides degradation. At 170 °C, the yield of arabinogalactans was found to be significantly higher than that of galactomannans (ηAG/ηGM >1). Increasing temperature to 200 °C leads to decrease the polymerization of polysaccharides, promoting the formation of debranched polysaccharides and oligosaccharides. This study shows that the optimum conditions for polysaccharides extraction cannot be selected only by mass yield but need to be defined according to the desired structural features for the specific applications.
Coffee brews have High Molecular Weight (HMW) compounds with described immunostimulatory activity, namely polysaccharides and melanoidins. Melanoidins are formed during roasting and are modified during brews technological processing. In addition, brews have Low Molecular Weight (LMW) compounds, namely free chlorogenic acids and caffeine, with well-known anti-inflammatory properties. However, this study shows that both espresso and instant coffee brews did not present immunostimulatory neither anti-inflammatory in vitro activities. It is possible that the simultaneous existence of compounds with antagonistic effects can mitigate their individual effects. To test this hypothesis, an ultrafiltration separation process was applied, studying the behavior of coffee brews’ HMW on retention of LMW compounds. Several ultrafiltration sequential cycles were required to separate retentates from LMW compounds, suggesting their retention. This effect was higher in instant coffee, attributed to its initial higher carbohydrate content when compared to espresso. Separation of HMW and LMW compounds boosted their immunostimulatory (6.2–7.8 µM nitrites) and anti-inflammatory (LPS induced nitrite production decrease by 36–31%) in vitro activities, respectively. As coffee anti-inflammatory compounds are expected to be first absorbed during digestion, a potential in vivo fractionation of LMW and HMW compounds can promote health relevant effects after coffee intake.
Single-dose coffee capsules have revolutionized the coffee market, fueling espresso coffee popularity and offering access to a wide selection of coffee blends. Nevertheless, scarce information related to coffee powder and brew’s combined volatile characterization is available. In this study, it is hypothesized that coffee brew aroma characteristics can be predicted based on coffee powder’s volatile composition. For this, headspace solid-phase microextraction (HS-SPME) combined with comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry detection (GC × GC-ToFMS) was used. The data were combined via chemometric tools to characterize in depth the volatile composition of eight blends of capsule-coffee powder and respective espresso brews, simulating the consumer’s perception. A total of 390 volatile compounds were putatively identified, 100 reported for the first time in roasted coffee or brews. Although the same chemical families were determined among the coffee powders and espresso brews, a different volatile profile was determined for each matrix. The Pearson correlation of coffee powders and respective brews allowed to identify 15 volatile compounds, mainly terpenic and esters recognized by their pleasant notes, with a strong relationship between the amounts present in both matrices. These compounds can be key markers to predict the volatile aroma potential of an espresso brew when analyzing the coffee powder.