Concept for the valorization of cereal processing waste: Recovery of phenolic acids by using waste-derived tetrahydrofurfuryl alcohol and biochar.

Valorization of agro-food waste by converting it into a renewable resource plays a crucial role in a bio-based circular economy. Therefore, this study was designed to evaluate the suitability of distillery stillage (DS), which comes from alcohol production from cereals, for producing value-added products that can be used synergistically. The main objective was to investigate the usefulness of two substances for the recovery of phenolic acids, which have antioxidant activity, from the liquid fraction of DS: namely, tetrahydrofurfuryl alcohol (THFA) as a solvent and biochar as an adsorbent, both produced from the solid fraction of cereal processing waste. The effect of THFA concentration (80 and 100%) on phenolic acid yield in ultrasound-assisted extraction was studied. The solubilization predictions of phenolic compounds by the Hansen solubility parameters were in accordance with the experimental results: the yield of phenolic acids in the extracts was highest (3.76 µg g-1 dry mass) with 80% THFA. Among the extracted phenolic acids, hydroxycinnamic acids predominated over hydroxybenzoic acids, which may affect the bioactive properties of the extracts and their future applications for industrial purposes. Phenolic acids from the extracts were adsorbed on 17-170 g biochar L-1 and desorbed into water at 40-60 °C. The phenolic acid recovery was highest (∼92%) when the biochar dose was 85 g L-1 and when desorption was performed at 50 °C. After adsorption/desorption, ∼95% of the antioxidant activity of the phenolic acids in the extracts was maintained. As biochar has a smaller specific surface area than commercial powdered activated carbon (PAC), the biochar dose should be about 5 times higher than an equivalent PAC dose for adsorption efficiency above 90%.

Valorization of distillery stillage by polyphenol recovery using microwave-assisted, ultrasound-assisted and conventional extractions.

An increasing understanding of the negative environmental effects of waste discharges has made valorization of distillery by-products to recover added-value compounds a sound option for distillery stillage management. In this study, the recovery of bioactive compounds, i.e. polyphenols, from distillery stillage was performed by microwave-assisted extraction (MAE), ultrasound-assisted extraction (UAE) and conventional solid-liquid extraction (CSLE) to investigate the effects of extraction time, the concentration of ethyl acetate (EA) in a solvent mixture with ethanol and water, and solid-to-solvent ratio on the recovery yield and antioxidant activity of the extracts. The highest yields of total polyphenol content (TPC) (3.73 mg gallic acid equivalent/g) and phenolic acid content (2.51 µg/g) were obtained with 8-min MAE with 70% EA. MAE provided 1.2- and 1.4-times higher yield of phenolic acids and 1.2- and 1.6-times higher antioxidant activity than UAE and CSLE, respectively. Due to the approximately 3-times higher rate of extraction, the ratio between energy consumption and extraction yield was better in MAE than in UAE. Principal component analysis (PCA) showed that the antioxidant activity of the extracts was positively correlated with TPC and phenolic acid content. Six phenolic acids that were identified were present mainly in their free forms (up to 95% of the total), with a predominance of ferulic (up to 0.80 µg/g) and p-coumaric (up to 0.72 µg/g) acids.

Processing of Distillery Stillage to Recover Phenolic Compounds with Ultrasound-Assisted and Microwave-Assisted Extractions.

This study investigated the effect of ultrasound-assisted extraction (UAE) and microwave-assisted extraction (MAE) conditions (extraction time, acetone concentration, solid-to-solvent ratio) on the efficiency of polyphenol recovery from distillery stillage and antioxidant activity of the extracts. The highest total polyphenol content, flavonoid content, and phenolic acid content were obtained with 10-min UAE and 5-min MAE at a solid-to-acetone ratio of 1:15 (w:v). Recovery yield was the highest with an aqueous solution of 60% acetone, confirming the results of Hansen Solubility Parameter analysis. Although UAE resulted in approximately 1.2 times higher extraction yield, MAE showed a better balance between extraction yield and energy consumption exhibited by its 3-fold higher extraction rate than that of UAE. Content of total polyphenols and phenolic acids strongly correlated with antioxidant activity, indicating that these compounds provide a substantial contribution to the bioactive properties of the extracts. Six phenolic acids were extracted, predominately ferulic and p-coumaric acids, and free forms of these acids constituted 91% of their total content, which opens various possibilities for their application in the food, cosmetics, and pharmaceutical industries.