Increasing the net value of forestry side-streams has both ecological as well as economic benefits for emerging biorefining industries. Spruce bark represents one of the nature’s abundant sources of valuable extractives. In this study, the impact of storage on the quality and quantity of Norway spruce (Picea abies) extractives was examined as a function of storage time, environmental conditions and season (i.e., winter or summer). The bark from stored spruce saw logs was extracted with an accelerated solvent extractor (ASE) at 120 °C with hexane and water. The produced extracts were analysed qualitatively and quantitatively by gas chromatography with a flame ionisation detector (GC-FID) and high-performance liquid chromatography (HPLC) methods. The total amount of phenolics in the water extracts was evaluated by the Folin–Ciocalteu method, while the carbohydrate and lignin content of the extractive-free bark was estimated by acidic hydrolysis and acidic methanolysis. According to the results, storage season and temperature dramatically influenced both the chemical composition and degradation rate of bark extractives. After a storage period of 24 weeks, the winter-stored saw log bark retained 22% more hydrophilic extractives than the summer-stored bark. Lipophilic extractives, however, were 14% higher during the summer. Notably, the average amount of monomeric stilbenoids was 61% higher during the winter storage period. The initial total phenolic content in the water extracts was significantly higher during winter, but the degradation rate was about equal during winter and summer. The amount of cellulose in dry bark decreased from 17% to 11% and from 13% to 6% during winter and summer, respectively. By contrast, hemicelluloses increased from 17% to 26% and 15% to 30% during winter and summer, respectively. Overall, it was demonstrated that the seasonal factors of storage greatly affected the degradation rate of valuable spruce bark extractives, which should be considered in the planning stages of the raw materials procurement chain.
Softwood bark is an important by-product of forest industry. Currently, bark is under-utilized and mainly directed for energy production, although it can be extracted with hot water to obtain compounds for value-added use. In Norway spruce (Picea abies [L.] Karst.) bark, condensed tannins and stilbene glycosides are among the compounds that comprise majority of the antioxidative extractives. For developing feasible production chain for softwood bark extractives, knowledge on raw material quality is critical. This study examined the fate of spruce bark tannins and stilbenes during storage treatment with two seasonal replications (i.e., during winter and summer). In the experiment, mature logs were harvested and stored outside. During six-month-storage periods, samples were periodically collected for chemical analysis from both inner and outer bark layers. Additionally, bark extractives were analyzed for antioxidative activities by FRAP, ORAC, and H2O2 scavenging assays. According to the results, stilbenes rapidly degraded during storage, whereas tannins were more stable: only 5–7% of the original stilbene amount and ca. 30–50% of the original amount of condensed tannins were found after 24-week-storage. Summer conditions led to the faster modification of bark chemistry than winter conditions. Changes in antioxidative activity were less pronounced than those of analyzed chemical compounds, indicating that the derivatives of the compounds contribute to the antioxidative activity. The results of the assays showed that, on average, ca. 27% of the original antioxidative capacity remained 24 weeks after the onset of the storage treatment, while a large variation (2–95% of the original capacity remaining) was found between assays, seasons, and bark layers. Inner bark preserved its activities longer than outer bark, and intact bark attached to timber is expected to maintain its activities longer than a debarked one. Thus, to ensure prolonged quality, no debarking before storage is suggested: outer bark protects the inner bark, and debarking enhances the degradation.
This study demonstrated the antibacterial and antiviral potential of condensed tannins and tannic acid when incorporated into fiber networks tested for functional material purposes. Condensed tannins were extracted from industrial bark of Norway spruce by using pressurized hot water extraction (PHWE), followed by purification of extracts by using XADHP7 treatment to obtain sugar-free extract. The chemical composition of the extracts was analyzed by using HPLC, GC‒MS and UHPLC after thiolytic degradation. The test matrices, i.e., lignocellulosic handsheets, were produced and impregnated with tannin-rich extracts, and tannic acid was used as a commercial reference. The antibacterial and antiviral efficacy of the handsheets were analyzed by using bioluminescent bacterial strains (Staphylococcus aureus RN4220+pAT19 and Escherichia coli K12+pCGLS11) and Enterovirus coxsackievirus B3. Potential bonding of the tannin-rich extract and tannic acid within the fiber matrices was studied by using FTIR-ATR spectroscopy. The deposition characteristics (distribution and accumulation patterns) of tannin compounds and extracts within fiber networks were measured and visualized by direct chemical mapping using time-of-flight secondary ion mass spectrometry (ToF-SIMS) and digital microscopy. Our results demonstrated for the first time, how tannin-rich extracts obtained from spruce bark side streams with green chemistry possess antiviral and antibacterial properties when immobilized into fiber matrices to create substitutes for plastic hygienic products, personal protection materials such as surgical face masks, or food packaging materials to prolong the shelf life of foodstuffs and prevent the spread of infections. However, more research is needed to further develop this proof-of-concept to ensure stable chemical bonding in product prototypes with specific chemistry.
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